HRID1088408

反应详情

EQUATION

反应方程式

HRID 1088408 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

40 Parts of cis-4-amino-5-chloro-N-[1-[3-(4-fluorophenoxy)propyl]-3-methoxy-4-piperidinyl]-2-methoxybenzamide monohydrate were boiled in 160 parts of methanol. The product was filtered off while hot and crystallized twice from a mixture of 600 parts of tetrachloromethane and 400 parts of trichloromethane. The product was filtered off, dried and recrystallized from 4-methyl-2-pentanone. The product was filtered off and dried (water-separator) yielding 18.5 parts of cis-4-amino-5-chloro-N-[2-chloro-4-[1-[3-(4-fluorophenoxy)propyl]-3-methoxy-4-piperidinyl]aminocarbonyl]-5-methoxyphenyl]-2--methoxybenzamide; mp. 181.5° C. (compound 239).

WORKUP

后处理

  1. filtrationThe product was filtered off while hot and
  2. customcrystallized twice from a mixture of 600 parts of tetrachloromethane and 400 parts of trichloromethane
  3. filtrationThe product was filtered off
  4. customdried
  5. customrecrystallized from 4-methyl-2-pentanone
  6. filtrationThe product was filtered off
  7. dry with materialdried (water-separator)