Process for the preparation of high-purity 1-(3-chloro-phenyl)-4

Details Process for the preparation of high-purity 1-(3-chloro-phenyl)-4 Process for the preparation of high-purity 1-(3-chloro-phenyl)-4

1992-05-04

1994-02-22

Ford, John M.

Organic compounds -- part of the class 532-570 series

Organic compounds

Unsubstituted hydrocarbyl chain between the ring and the -c-...

C07D24302

Patent

active

052888630

ABSTRACT:
The invention relates to a process for the preparation of 1-(3-chlorophenyl)-4-methyl-7,8-dimethoxy-5 H-2,3-benzodiazepine of formula (I) ##STR1## in high purity and in a quality suitable for pharmaceutical purposes. According to the invention the reaction of 1 mole of 2-acetonyl-3'-chloro-4,5-dimethoxybenzophenone of formula (II) ##STR2## with 3-7 moles of hydrazine hydrate in an organic solvent or in a mixture of organic solvents at a temperature between 15.degree. C. and 85.degree. C. is carried out in the absence of air oxygen, optionally in the presence of water. The crude product is then recrystallized from an aliphatic alcohol containing 1 to 5 carbon atom(s).

REFERENCES:
patent: 4322346 (1982-03-01), Korosi et al.
Lang, Chemical Abstract 105:133915k (1986).
Korosi, Chemical Abstract 93:168318d (1980).
Christian et al., editors, Instrumental Analysis, 2nd ed. (1978), p. 56, (Allyn and Bacon, Inc.).
Kirk-Othmer Encyclopedia of Chemical Technology, 3rd ed. (1981), p. 939, (John Wiley and Sons).

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