HRID236778

反应详情

EQUATION

反应方程式

HRID 236778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 5.5 parts of 4-(methoxymethyl)-1-(1-methylethyl)-N-phenyl-4-piperidinamine in 56 parts of benzene is added dropwise a solution of 13.8 parts of benzeneacetyl chloride in 45 parts of benzene at 26°-32° C. Upon completion, stirring is continued first for one hour at 26°-32° C. and further for 3.60 hours at 38°-55° C. After cooling, the precipitated product is filtered off and converted into the hydrochloride salt in a mixture of 2-propanol and 2-propanone (5:1 by volume). The salt is filtered off and dissolved in absolute ethanol. After standing for 72 hours at room temperature, the precipitated product is filtered off, washed with a small amount of 2-propanone and dried, yielding 1.05 parts of N-[4-(methoxymethyl)-1-(1-methylethyl)-4-piperidinyl]-N-phenylbenzeneacetamide hydrochloride; mp. 249.1° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe precipitated product is filtered off
  3. additionconverted into the hydrochloride salt in a mixture of 2-propanol and 2-propanone (5:1 by volume)
  4. filtrationThe salt is filtered off
  5. dissolutiondissolved in absolute ethanol
  6. waitAfter standing for 72 hours at room temperature
  7. filtrationthe precipitated product is filtered off
  8. washwashed with a small amount of 2-propanone
  9. customdried