HRID357590

反应详情

EQUATION

反应方程式

HRID 357590 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 157 mg (1.0 mmol) of 4-cyano-2,3-dihydro-1H-inden-1-one [Coll. Czechoslov. Chem. Commun. 43, 3227 (1978)] and 139 mg (2.0 mmol) of hydroxylamine hydrochloride in 4 ml of ethanol is stirred at 80° C. for 1.5 hours and cooled in an ice-water bath. The product that has crystallized out is filtered off with suction, washed with cold ethanol and diethyl ether and dried. In that manner there is obtained the intermediate 4-cyano-2,3-dihydro-1H-inden-1-one oxime, which melts at 200°-202° C. with decomposition; 1H-NMR (DMSO): δ=11.22 (s, 1H); 7.84 (d, 1H); 7.81 (d, 1H); 7.45 (t, 1H); 3.15 (t, 2H); 2.84 (t, 2H).

WORKUP

后处理

  1. temperaturecooled in an ice-water bath
  2. customThe product that has crystallized out
  3. filtrationis filtered off with suction
  4. washwashed with cold ethanol and diethyl ether
  5. customdried