HRID567931

反应详情

EQUATION

反应方程式

HRID 567931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 g (3.5 mmol) of methyl 3-nitryloxy-2,2-bis(nitryloxymethyl)propionate is heated for 3 hours at 130° C. with 3 ml of benzylamine and 100 mg of ammonium chloride and the mixture is cooled, taken up in 50 ml of chloroform and washed successively with water, with dilute hydrochloric acid, with aqueous bicarbonate solution and again with water. The crude product obtained after evaporation of the solvent is purified by column chromatography to give 3-nitryloxy-2,2-bis(nitryloxymethyl)propionic acid N-benzylamide (Tri-PA-NBzl amide) as a colourless oil. Yield: 73%. Elemental analysis: (C: conforms, H: conforms, N: conforms).

WORKUP

后处理

  1. temperaturethe mixture is cooled
  2. washwashed successively with water, with dilute hydrochloric acid, with aqueous bicarbonate solution and again with water
  3. customThe crude product obtained
  4. customafter evaporation of the solvent
  5. customis purified by column chromatography