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    METHOD FOR THE PREPARATION OF THE MONOPOTASSIUM SALT OF 1, 2, 5-THIADIAZOL-3,4-DICARBOXYLIC ACID, AND INTERMEDIATE PRODUCT
    25.
    发明专利
    METHOD FOR THE PREPARATION OF THE MONOPOTASSIUM SALT OF 1, 2, 5-THIADIAZOL-3,4-DICARBOXYLIC ACID, AND INTERMEDIATE PRODUCT 未知

    公开(公告)号：CA1083580A

    公开(公告)日：1980-08-12

    申请号：CA273985

    申请日：1977-03-15

    Applicant: MONTEDISON SPA

    Inventor： RIBALDONE GIUSEPPE ,  GRECU RENATO

    IPC: C07D285/10

    Abstract: : Process for the preparation of the monopotassium salt of 1,2,5-thiadiazol-3,4-dicarboxylic acid (I). Involves double-stage saponification of 3,4-dicyano-1,2,5-thiadiazole (II), 3-cyano-4-carboamoyl-1,2,5-thiadiazole (III) is obtained from an aqueous suspension of 3,4-dicyano-1,2,5-thiadiazole (II) by catalytic hydration through the addition of aqueous KOH, desirably at a temperature of from 20.degree. to 50.degree.C. and with a molar ratio of 3,4-dicyano-1,25-thiadiazole (II) to KOH of from 1:0.01 and 1:0.8. This is followed by hydrolysis, by the further addition of aqueous KOH, desirably at a temperature of from 85 to 100.degree.C, until attaining an overall molar ratio of 3,4-dicyano-1,2,5-thiadiazole (II) to KOH of from about 1:2.0 and 1:2.35, a molar ratio of 3,4-dicyano-1,2,5-thiadiazole (II) to H20 of from about 1:20 to 1:23. Thereafter, from the resulting solution of dipotassium salt of 1,2,5-thiadiazole-3,4-diccarboxylic acid, the monopotassium salt is separated by acidification of said solution.

    28.
    发明专利
    未知

    公开(公告)号：DE2254502A1

    公开(公告)日：1973-05-17

    申请号：DE2254502

    申请日：1972-11-08

    Applicant: MONTEDISON SPA

    Inventor： RIBALDONE GIUSEPPE ,  BORSOTTI GIAMPIERO

    IPC: C07C20060101 ,  C07C255/30 ,  C09B20060101 ,  C07C121/70

    Abstract: A process for the preparation of compounds having the formula: ** (see formula) ** Wherein r is a hydrogen atom or the methyl group, characterized in that an N-ethyl-amino-benzene selected from N-ethyl-aniline and N-ethyl-m-toluidine is reacted with 1,4-dichloro-2-butene, according to a trans-1,4-dichloro-2-butene/n-ethyl-amino-benzene molar ratio equal to at least 5, at a temperature between 20º and 120ºC already the atmospheric pressure, in the presence of a neutralizing agent; by the fact that the reaction mass thus obtained is subjected to a first extraction with 0.5 normal hcl, selective for the extraction of the unreacted N-ethyl-benzene-benzene and of the di-substitution product, and the residue subjected to a second extraction with normal 2 hcl, selective for N-ethyl-N- (2-butene-4-chloro) -amino-benzene; due to the fact that from the normal hydrochloric acid solution thus obtained, N-ethyl-N- (2-butene-4-chloroaniline or, respectively, N-ethyl-n) are isolated after neutralization. - (2-butene-4-chloro) -m-toluidine according to known techniques, and are then transformed by cyanidation into N-ethyl-N- (2-butene-4-cyano) -aniline or, respectively, N- ethyl-N- (2-butene-4-cyano) -m-toluidine. (Machine-translation by Google Translate, not legally binding)

    PROCESS FOR THE PREPARATION OF NITRILOTRIACETONITRILE
    29.
    发明专利
    PROCESS FOR THE PREPARATION OF NITRILOTRIACETONITRILE 未知

    公开(公告)号：GB1294674A

    公开(公告)日：1972-11-01

    申请号：GB6056569

    申请日：1969-12-11

    Applicant: MONTEDISON SPA

    Inventor： RIBALDONE GIUSEPPE ,  GAFA SALVATORE ,  AGAMENNONE MARCO ,  BORSOTTI GIAMPIERO

    IPC: C07C255/25

    Abstract: 1294674 Nitrilotriacetonitrile MONTECATINI EDISON SpA 11 Dec 1969 [11 Dec 1968] 60565/69 Heading C2C Nitrilotriacetonitrile N(CH 2 CN) 3 is prepared by reacting an aqueous mixture of formaldehyde, ammonia and sulphuric acid in which the ratio of HCHO : NH 3 : H 2 SO 4 is in the range 3 : 1À05-1À15 : 0À37-0À40, particularly 3 : 1.1 : 0.385, with liquid HCN at a temperature from 40-100‹ C., said HCN being continuously fed into the aqueous mixture in an amount in an excess of that required to maintain it at saturation concentration in the mxiture under' the reaction conditions. The preferred water content of the aqueous mixture corresponds to a molar ratio of HCHO : H 2 O of from 3 : 7 to 3 : 20, particularly between 3 : 8 and 3 : 10. The reaction may be effected in two or more stages, the first at 50-70‹ C.. and the second (and any further stages) at progressively higher temperatures in the range 70-90‹ C. Preferred reaction times are 10-20 minutes for the first stage, and from 20-40 minutes for each subsequent stage.

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