HRID1764117

反应详情

EQUATION

反应方程式

HRID 1764117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 79 g (1.14 mole) of hydroxylamine hydrochloride in 770 ml of H2O, contained in a 2 l. Erlenmeyer flask, was treated with 619 ml of 10% NaOH, 150 g (0.78 mole) of 6-nitro-4-chromanone and enough ethanol (750 ml) to produce a solution at the boiling point. The reaction mixture was boiled for 25 min., cooled to 50° over 2 hrs., and filtered. The filtrate was refrigerated overnight and filtered. The tan crystalline solid was washed with 200 ml of ethanol and dried, m.p. 173°-178°. Yield: 60 g (37%).

WORKUP

后处理

  1. customto produce a solution at the boiling point
  2. temperaturecooled to 50° over 2 hrs
  3. filtration, and filtered
  4. waitThe filtrate was refrigerated overnight
  5. filtrationfiltered
  6. washThe tan crystalline solid was washed with 200 ml of ethanol
  7. customdried