HRID1449058

反应详情

EQUATION

反应方程式

HRID 1449058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.6 Parts of finely ground sodium hydroxide is added to a suspension of 3 parts of 1-[(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)methyl]-4-piperidinone and 1.5 part of hydroxylamine hydrochloride in 50 parts by volume of ethanol-water (4:1) solution. The resultant mixture is heated on a steam bath for about 5 hours and then partitioned between water and ethyl acetate. The aqueous layer is separated and extracted with a second portion of ethyl acetate. The ethyl acetate extracts are combined, dried, and concentrated to give 1-[(10,11-dihydro-5H-dibenzo[a,d]-cyclohepten-5-yl)methyl]-4-piperidinone oxime, as a white solid which melts at about 199°-202° C. after recrystallization from dioxane. This compound is represented by the following structural formula ##STR33##

WORKUP

后处理

  1. custompartitioned between water and ethyl acetate
  2. customThe aqueous layer is separated
  3. extractionextracted with a second portion of ethyl acetate
  4. customdried
  5. concentrationconcentrated