PRODUCTION OF TETRAHYDROBENZYL ALCOHOL OR VINYLYSLOHEXENE

    公开(公告)号:JPH06172238A

    公开(公告)日:1994-06-21

    申请号:JP32821392

    申请日:1992-12-08

    Applicant: DAICEL CHEM

    Abstract: PURPOSE:To obtain a method for producing tetrahydrobenzyl alcohol or vinylcyclohexene with minimized amount of by-produced butadiene polymer to a loss of a raw material. CONSTITUTION:This method for producing tetrahydrobenzyl alcohol or vinylcyclohexane comprises effecting the reaction in the coexistence of a metallic alkoxide in an amount of =5kg/cm pressure in synthesizing the tetrahydrobenzyl alcohol by the Diels- Alder reaction of butadiene with allyl alcohol or the vinylcyclohexene by the Diels-Alder reaction of the butadiene.

    PRODUCTION OF 2,2,4,4,6-PENTAMETHYL-2,3,4,5-TETRAHYDROPYRIMIDINE

    公开(公告)号:JPH0395163A

    公开(公告)日:1991-04-19

    申请号:JP23331089

    申请日:1989-09-08

    Applicant: DAICEL CHEM

    Inventor: SHIMADA GIICHI

    Abstract: PURPOSE:To obtain the subject compound as a stabilizer for synthetic polymer materials or intermediate for medicines, etc., in high yield for a short time without using a corrosion-resistant material and forming by-products by reacting acetone with ammonia using an iron carboxylate catalyst. CONSTITUTION:Acetone and/or an acidic condensate thereof and ammonia are reacted in the presence of an iron carboxylate catalyst in an amount of 0.05-10mol%, preferably 0.1-10mol% based on the acetone and/or acidic condensate thereof at 0-60 deg.C, preferably 10-25 deg.C to afford the objective compound. Furthermore, acetic acid, lactic acid, oxalic acid, citric acid, etc., are preferred as the aforementioned carboxylic acid. Diacetone alcohol, mesityl oxide, etc., are cited as the acetone or acidic condensate of the acetone used with the acetone in combination.

    PURIFICATION OF ISOPHORONE
    15.
    发明专利

    公开(公告)号:JPS61289055A

    公开(公告)日:1986-12-19

    申请号:JP13109385

    申请日:1985-06-17

    Applicant: DAICEL CHEM

    Abstract: PURPOSE:To obtain colorless and stable isophorone with simple procedure, by contacting a crude isophorone liquid (an oil layer) with a specific ion exchange resin to decrease the concentration of the alkaline substance in the oil layer to the permissible level, and purifying the liquid by vacuum distillation. CONSTITUTION:Crude isophorone liquid (an oil layer) produced by the alkali condensation of acetone is made to contact with a weakly acidic anion exchange resin [e.g. Diaion WK11 (product of Mitsubishi Chemical Co.)] at room temperature (20-50 deg.C) to decrease the concentration of residual alkaline substance in the treated isophorone to 20ppm, and the treated product is refined by vacuum distillation to obtain the objective colorless and clear isophorone having high stability. Any resin having excellent solvent resistance to isophorone and capable of adsorbing an alkali ion such as Na in a solution may be used as the above ion exchange resin. The resin can be regenerated easily. EFFECT:A stable product storable keeping colorless and transparent state can be produced.

    Preparation of crotonic acid
    16.
    发明专利
    Preparation of crotonic acid 失效
    CROTONIC酸的制备

    公开(公告)号:JPS5762238A

    公开(公告)日:1982-04-15

    申请号:JP13834580

    申请日:1980-10-03

    CPC classification number: Y02P20/52

    Abstract: PURPOSE: To prepare crotonic acid useful in varius fields such as synthetic resin, plasticizer, etc., in high yield and selectvity, by oxidizing crotonaldehyde with a percaboxylic acid in the presence of a specific amount of a soluble manganese salt of an organic acid as a catalyst.
    CONSTITUTION: Crotonic acid is prepaed by oxidizing crotonaldehyde with a per- carboxylic acid such as peracetic acid, perpropionic acid, perisobutyric acid, etc. in the presence of a soluble manganese salt of an organic acid such as caroxylic acid, thiocyanic acid, etc., pref. at 10W40°C. The amount of the manganese salt is 0.1W1.0wt% as manganese based on crotonaldehyde. Crotonic acid has high re- activity of unsaturated fatty acid, and is an industrially important compound having a number of potential application fields such as lubricant additive, insecticide, per- fume, pharmaceutical, lacquer solvent, etc. as well as the above actual applications.
    COPYRIGHT: (C)1982,JPO&Japio

    Abstract translation: 目的:通过在特定量的有机酸的可溶性锰盐的存在下,以高产率和可选择性制备用于各种领域的巴豆酸,例如合成树脂,增塑剂等,通过用过羟酸酸化巴豆醛, 催化剂 构成:通过在诸如过氧乙酸,过丙酸,过碘酸等的有机酸的可溶性锰盐如羧酸,硫氰酸等的存在下,用过羧酸氧化巴豆醛来制备巴豆酸。 ,pref。 在10-40℃ 锰盐的量为以巴豆醛为代表的锰的0.1〜1.0重量%。 巴豆酸具有高不饱和脂肪酸的再活性,是具有许多潜在应用领域的工业上重要的化合物,如润滑添加剂,杀虫剂,香料,药物,漆溶剂等,以及上述实际应用 。

    PRODUCTION OF ISOPROPYL ACETATE
    17.
    发明专利

    公开(公告)号:JPH072735A

    公开(公告)日:1995-01-06

    申请号:JP34006393

    申请日:1993-12-07

    Abstract: PURPOSE:To obtain isopropyl acetate from crude propylene and acetic acid by a liquid phase reaction; firstly separating a low-boiling point component from a pressurized crude reaction solution, secondly separating the objective material, thereafter separating the unreacted material and a high-boiling point component and recycling the unreacted material to the reaction. CONSTITUTION:High purity isopropyl acetate is obtained by the following processes. A catalyst consisting of acidic ion exchange resin is placed in a reaction vessel 1 and an impurity-containing propylene and acetic acid are supplied to the reaction vessel 1. The pressurized reactional solution obtained by the reaction in the reaction vessel 1 is depressurized in a flush tank 2 to separate into a vapor phase and a liquid phase. The vapor phase is cooled in a condenser 3 and the condensate is mixed, in a tank 4, with the liquid phase obtained above. The mixed crude reactional solution is introduced into the first distillation tower 5, a low-boiling point component is condensed and removed and the remainder is treated in the third distillation tower 7 to obtain the objective product of isopropyl acetate. The remainder of the third distillation tower 7 is further treated in the fourth distillation tower 8 and a mixture consisting of unreacted acetic acid and sec-butyl acetate is taken out by side cut and returned to the reaction. The bottom of the fourth distillation tower 8 is removed from the reaction system.

    PRODUCTION OF 2,2,6,6-TETRAMETHYL-4-OXOPIPERIDINE

    公开(公告)号:JPH03188065A

    公开(公告)日:1991-08-16

    申请号:JP20838689

    申请日:1989-08-11

    Applicant: DAICEL CHEM

    Inventor: SHIMADA GIICHI

    Abstract: PURPOSE:To obtain the subject substance in high yield in a short time while producing little by-product by reacting acetone or an acidic condensate of acetone with 2,2,4,4,6-pentamethyl-2,3,4,5-tetrahydropyrimidine in the presence of an iron carboxylic acid salt as a catalyst. CONSTITUTION:The subject substance can be produced by reacting acetone or an acidic condensate of acetone (e.g. diacetone alcohol) with a compound of formula at about 60 deg.C for 5-10hr in the presence of a carboxylic acid iron salt as the reaction catalyst. The carboxylic acid constituting the catalyst is preferably acetic acid, oxalic acid, lactic acid, citric acid, etc., and the amount of the catalyst is preferably 0.01-0.2mol per 1mol of the compound of formula. The above catalyst may be used in combination with a Lewis acid, protonic acid, etc. The subject substance useful as a photo-stabilizer for polymeric material or synthetic intermediate for pharmaceuticals, etc., can be produced in colorless state by the above process in high yield.

    PRODUCTION OF ODORLESS DIGLYCEROL
    19.
    发明专利

    公开(公告)号:JPH01254636A

    公开(公告)日:1989-10-11

    申请号:JP8354688

    申请日:1988-04-05

    Applicant: DAICEL CHEM

    Abstract: PURPOSE:To obtain odorless diglycerol neither emitting an offensive smell nor causing precipitate when used as an esterified substance or etherified substance for cosmetic, etc., by hydrogenating purified diglycerol in the presence of water and a reducing catalyst, separating the catalyst and dehydrating. CONSTITUTION:Crude liquid of diglycerol prepared as a by-product in production of synthetic glycerol is purified to give purified glycerol, which is reduced in the presence of water by using a reducing catalyst so that polymers of triglycerol and polyglycerols existing as impurities are previously hydrolyzed and aldehydes such as acrolein caused by the hydrolysis are reduced to remove substances to cause an offensive smell and precipitate are removed. Then the catalyst is removed and the purified diglycerol is dehydrated to give odorless diglycerol whose esterified substance and etherified substance are useful as cosmetic additives to humectant, softening agent for the skin, etc.

    PRODUCTION OF GLUTARALDEHYDE MONOACETAL

    公开(公告)号:JPH11302274A

    公开(公告)日:1999-11-02

    申请号:JP3818899

    申请日:1999-02-17

    Applicant: DAICEL CHEM

    Abstract: PROBLEM TO BE SOLVED: To obtain the subject compound from a dihydropyran and a diol in a high yield by reacting two specific kinds of by-products produced by a reaction. SOLUTION: A 2-Y-3,4-dihydro-2H-pyran of formula I (Y is hydroxy, an alkoxy or the like) or its nuclear substituent derivative is reacted with a dial of the formula; HO-R-OH (R is a 1-10C bifunctional saturated or unsaturated hydrocarbon) (preferably ethylene glycol or the like) to give the objective compound of formula II. Further glutaraldehyde (GA) of formula III as one by- product is reacted with glutaraldehyde bisacetal (BADBA) of formula IV as another by-product to give the objective compound. After the reaction of the compound of formula I and the dial, preferably a low-boiling fraction containing GA and a high-boiling fraction containing GADBA are separated from the crude reaction solution by distillation. Preferably the separation of the GA- containing fraction is carried out at 130-142 deg.C distillation column still temperature under 25-35 Torr column top pressure at 95-119 deg.C column top temperature.

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