HRID2106748

反应详情

EQUATION

反应方程式

HRID 2106748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.6 parts of N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-4-phenyl-2-thiazolamine, 2 parts of bromoethane, 1 part of sodium hydroxide and 94 parts of N,N-dimethylformamide was stirred for 16 hours at room temperature. Another portion of 2 parts of bromoethane and 1 part of sodium hydroxide was added and stirring was continued for 4 hours at 50° C. The reaction mixture was diluted with water. The precipitated product was filtered off and purified by column chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 4-methyl-2-pentanone. The product was filtered off and dried, yielding 4.0 parts (81.7%) of N-ethyl-N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-4-phenyl-2-thiazolamine; mp. 223.6° C. (int. 3).

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 4 hours at 50° C
  3. filtrationThe precipitated product was filtered off
  4. custompurified by column chromatography over silica gel
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated
  7. customThe residue was crystallized from 4-methyl-2-pentanone
  8. filtrationThe product was filtered off
  9. customdried