公开(公告)号：JPH11130708A

公开(公告)日：1999-05-18

申请号：JP29829597

申请日：1997-10-30

Applicant: TOSOH CORP

Inventor： AWANO YUTAKA ,  SHIMODA ATSUSHI ,  KUBO MASAJI

IPC: B01J31/02 ,  C07B39/00 ,  C07B61/00 ,  C07C17/14 ,  C07C22/08 ,  C07C25/02 ,  C07C63/70 ,  C07C201/12 ,  C07C205/11 ,  C07C255/50

Abstract: PROBLEM TO BE SOLVED: To provide a method for producing a monobromomethylated aromatic compound, capable of solving a problem that the selectivity of the monobromomethylated product is low by conventional methods, and capable of efficiently obtaining the monobromomethylated aromatic compound by an industrially simple method without using a special device such as a photoreactor or the like. SOLUTION: This method for producing a monobromomethylated aromatic compound comprises brominating a methyl group bound to the aromatic ring of a substituted aromatic compound of the formula (R is at least one electron- attracting substituent selected from nitro group, a halogen atom, trifluoromethyl group, cyano group, carboxyl group, an alkoxycarbony group and phenoxy group). Therein, the reaction is carried out in the presence of water and one or more kinds of radical initiators selected from the group consisting of dialkyl peoxides, diacyl peroxide and azo compounds.

公开(公告)号：JPH049346A

公开(公告)日：1992-01-14

申请号：JP10891590

申请日：1990-04-26

Applicant: TOSOH CORP

Inventor： EGUCHI HISAO ,  KUBO MASAJI ,  NAGASAKI YORITAKA ,  KUNIMOTO KOJI

IPC: C07C37/86 ,  C07C37/62 ,  C07C37/84 ,  C07C39/16 ,  C07C39/367

Abstract: PURPOSE:To obtain the title high-quality compound reduced in hydrolyzable bromine and inorganic bromide ion contents by bromination of bisphenol A with bromine followed by adding a specified amount of water at a specified dripping rate to the reaction fluid to effect crystallization. CONSTITUTION:Firstly, bisphenol A is incorporated, in a methanol solvent, with 4.0-4.5 molar times of bromine at 10-30 deg.C for 0.5-10hr to effect bromination followed by aging the system for 0.5-5hr. Thence, 30-100 (pref. 50-85)wt.%, based on the reaction solvent, of water is added to the system at a dripping rate of 5-40 (pref. 10-30)wt.%/hr, thus obtaining the objective high-quality compound containing only 5-50ppm of hydrolyzable bromine and 0-10ppm of inorganic bromide ion. The present compound can be directly used as a flame-retardant for the resins to be used as electrical/electronic materials such as laminates and sealers.

公开(公告)号：JPH0331183B2

公开(公告)日：1991-05-02

申请号：JP20111983

申请日：1983-10-28

Applicant: TOSOH CORP

Inventor： KUBO MASAJI ,  SATSUKA HIDEO ,  TSUTSUMI YUKIHIRO

IPC: C07C17/392 ,  C07C17/00 ,  C07C17/38 ,  C07C25/18 ,  C07C25/22 ,  C07C67/00

公开(公告)号：JP2005330189A

公开(公告)日：2005-12-02

申请号：JP2004147408

申请日：2004-05-18

Applicant: Tosoh Corp ,  東ソー株式会社

Inventor： TACHI NORITOMO ,  KUBO MASAJI

IPC: C07D307/33 ,  C07B61/00

Abstract: PROBLEM TO BE SOLVED: To provide an inexpensive and simple method for producing β-hydroxy-γ-butyrolactone.
SOLUTION: A vinylacetic acid represented by general formula (1) is reacted with hydrogen peroxide in the presence of an acid catalyst having a sulfonic acid group to afford the β-hydroxy-γ-butyrolactone represented by general formula (2).
COPYRIGHT: (C)2006,JPO&NCIPI

Abstract translation: 待解决的问题：提供生产β-羟基-γ-丁内酯的廉价且简单的方法。 解决方案：通式（1）表示的乙烯基乙酸在具有磺酸基的酸催化剂存在下与过氧化氢反应，得到通式（2）所示的β-羟基-γ-丁内酯。 版权所有（C）2006，JPO＆NCIPI

公开(公告)号：JPH10310562A

公开(公告)日：1998-11-24

申请号：JP8049598

申请日：1998-03-13

Applicant: TOSOH CORP

Inventor： NAGAI RYUICHIRO ,  KUBO MASAJI ,  AWANO YUTAKA ,  MIYANO OSAMU

IPC: C07C209/08 ,  C07C211/63

Abstract: PROBLEM TO BE SOLVED: To obtain the subject compound large in the diameters of its crystals and useful as an intermediate for synthesizing dyestuffs, agrochemicals, medicines, etc., in a high yield and in a high purity by reacting a benzyl bromide with hexamethylenetetramine and subsequently hydrolyzing the obtained ammonium salt in the presence of an acid in an alcohol-water mixture solvent. SOLUTION: This method for producing a benzylamine salt of formula II (M is a counter ion of n-valent benylammonium ion) comprises thermally reacting a benzyl bromide of formula I (R is H, a halogen, trifluoromethyl, etc.) such as benzyl bromide or 2-bromobenyzl bromide with the equivalent amount of hexamethylenetetramine, hydrolyzing the obtained quaternary ammonium salt in the presence of an acid, e.g. an inorganic acid such as hydrochloric acid, nitric acid or sulfuric acid in the water mixture solvent with a low boiling point alcohol such as methanol, ethanol or propanol preferably at 15-50 deg.C, filtering off the generated crystals and subsequently washing the obtained crystals with water or a diluted acid.

公开(公告)号：JPH0482849A

公开(公告)日：1992-03-16

申请号：JP19504390

申请日：1990-07-25

Applicant: TOSOH CORP

Inventor： ODA YASUHIRO ,  YOSHIMITSU MITSUAKI ,  KUBO MASAJI

IPC: B01D15/00 ,  C07C17/38 ,  C07C17/389 ,  C07C25/28

Abstract: PURPOSE:To enable effective decoloration of a colored nucleus-brominated styrene on an industrial scale at a low cost by dissolving the crude brominated styrene in an aliphatic hydrocarbon and contacting with a specific adsorbent such as oxides composed mainly of silica or alumina. CONSTITUTION:A colored nucleus-brominated styrene (BS) is dissolved in a cyclic or chain saturated aliphatic hydrocarbon having a carbon number of about 5-8 (especially hexane, heptane or octane) and made to contact with one or more kinds of adsorbents selected from (a) oxide composed mainly of silica or alumina, (b) carbonate, phosphate or silicate of calcium or magnesium and (c) amorphous carbon. The BS can effectively be decolored by this process. A BS which does not cause discoloration of a resin molded article after polymerization, especially mono-to tribromostyrene useful as a reactive flame-retardant or monomer for a polymeric material can be produced with a simple procedure by a process having high industrial utilization value and practicability at a low cost.

公开(公告)号：JPH0441473A

公开(公告)日：1992-02-12

申请号：JP14449490

申请日：1990-06-04

Applicant: TOSOH CORP

Inventor： SAKKA HIDEO ,  KUBO MASAJI

IPC: C07C315/04 ,  C07C317/22

Abstract: PURPOSE:To obtain the subject compound in high yield and high purity by reacting bis(4-hydroxy-3,5-dibromophenyl) sulfone with allyl chloride, separating and recovering an intermediate from reaction product in a solution state and circulating to the reaction process. CONSTITUTION:Bis(4-hydroxy-3,5-dibromophenyl) sulfone is reacted with allyl chloride in an uniform aqueous solution mixed with a water-soluble organic solvent (preferably isopropanol or dioxane) in the presence of alkali and resul tant slurry solution is distilled to reduce concentration of the organic solvent to

公开(公告)号：JPH03271267A

公开(公告)日：1991-12-03

申请号：JP6839890

申请日：1990-03-20

Applicant: TOSOH CORP

Inventor： SAKKA HIDEO ,  EGUCHI HISAO ,  KUBO MASAJI

IPC: C07C315/04 ,  C07C315/06 ,  C07C317/22

Abstract: PURPOSE:To obtain the subject substance in high yield by adding a specific solvent to an aqueous solution of alkaline slurry of a product derived from allylation reaction of bis(4-hydroxy-3,5-dibromophenyl) sulfone, selectively extracting the product and subjecting to a bromination process. CONSTITUTION:Bis(4-hydroxy-3,5-dibromophenyl) sulfone is used as a raw material and subjected to allylation reaction. Then, a halogenated hydrocarbon solvent (especially methylene chloride is preferable) is added to an aqueous solution of alkaline slurry of resultant bis(4-allyloxy-3,5-dibromophenyl) sulfone so as substrate concentration of the product to be in a range of 5-25wt.%. Subsequently, resultant bis(4-allyloxy-3,5-dibromophenyl) sulfone is selectively extracted into an organic phase and separated, then bromine is added to the organic phase, thus reacted to afford the aimed compound. Said compound is useful as a flame retarder of polyolefin resin, etc.

公开(公告)号：JPH03246245A

公开(公告)日：1991-11-01

申请号：JP4120690

申请日：1990-02-23

Applicant: TOSOH CORP

Inventor： EGUCHI HISAO ,  KUBO MASAJI ,  KUNIMOTO KOJI

IPC: C07C37/62 ,  C07C37/84 ,  C07C39/367

Abstract: PURPOSE:To obtain the objective high-quality compound by adding water to a reaction solution after completing brominating reaction and crystallizing the objective compound in brominating bisphenol A with bromine in a methanolic solvent and producing the subject compound. CONSTITUTION:Bisphenol A is brominated in a methanolic solvent to produce tetrabromobisphenol A useful as a reactive type flame retardant for epoxy resins. In the process, water is added to the reaction solution after completing the brominating reaction to crystallize the objective compound at -15 to +15 deg.C temperature. Thereby, the objective high-quality compound with a remarkably reduced content of hydrolyzable bromine or inorganic bromine ions causing metal corrosion, etc., deterioration in reliability of materials in use thereof as the epoxy resins for electrical and electronic material applications such as especially laminated boards or sealing media is advantageously and industrially obtained in a simplified process without requiring special purifying steps.

公开(公告)号：JPH03232827A

公开(公告)日：1991-10-16

申请号：JP28845390

申请日：1990-10-29

Applicant: TOSOH CORP

Inventor： MATSUBA TAKAO ,  KUBO MASAJI ,  KAWAHATA KOUJI

IPC: C07C17/02 ,  C07C23/02

Abstract: PURPOSE:To obtain the gamma-modification of the title compound in high selectivity through reaction between bromine and 1,5,9-cis, trans, trans-cyclododecatriene in the presence of an alcoholic solvent by making the substrate concentration based on the solvent fall within a specified range. CONSTITUTION:The gamma-modification of the title compound can be obtained in high selectivity by reaction between bromine and (A) 1,5,9-cis, trans, trans- cyclododecatriene in the presence of a 1-4C alcohol or an organic solvent containing the same at the substrate concentration for the compound A based on the solvent falling between 0.1 and 20w/v%. The amount of the bromine to be used is pref. e.g. 3.0-10.0 in the molar ratio Br2/the compound A, and the reaction should be carried out at -2050 deg.C. Compared to the reaction processes with higher substrate concentrations, the production of the impurities derived from the compound A will be significantly reduced, leading to the objective compound with excellent hue and thermal stability. The title compound is useful as a flame retardant for polymers.