HRID1076185

反应详情

EQUATION

反应方程式

HRID 1076185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under cooling, a solution of 200 mg. of hydroxylamine in 15 ml. of ethanol is combined with 10 ml. of a sodium ethylate solution containing 1% sodium, as well as, in incremental portions, with 1.0 g. of the ethyl ester of 7-chloro-8-methylcarbazole-1-carboxylic acid. The mixture is stirred for one hour at 0° C. and for another 12 hours at room temperature and is then concentrated under vacuum. The residue is taken up in water, acidified to pH 1 with hydrochloric acid, extracted with ethyl acetate, and the extract is washed and concentrated. The residue is recrystallized from ethanol - water, thus obtaining in a 20% yield, 7-chloro-8-methylcarbazole-1-carbohydroxamic acid, m.p. 200° C.

WORKUP

后处理

  1. temperatureUnder cooling
  2. concentrationis then concentrated under vacuum
  3. extractionextracted with ethyl acetate
  4. washthe extract is washed
  5. concentrationconcentrated
  6. customThe residue is recrystallized from ethanol - water