HRID2102297

反应详情

EQUATION

反应方程式

HRID 2102297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

27.2 g crude N′-[(3-chlorobenzoyl)oxy]-2-hydroxypropanimidamide was dissolved in ethanol (250 mL) and refluxed for 1 h, followed by addition of 14.0 g (170 mmol) sodium acetate in water (40 mL). After refluxing o.n., cooling to r.t. and addition of water (250 mL) the mixture was concentrated in vacuo to about ½ of its volume, resulting in a precipitate which was filtered off and recrystallized from EA/Hep to yield 6.45 g (25%) of the title compound. 1H NMR: 8.14 (s, 1H), 8.02 (d, 1H), 7.57 (d, 1H), 7.47 (t, 1H), 5.04 -5.14 (m, 1H), 2.51 (d, 1H), 1.67 (d, 3H)

WORKUP

后处理

  1. temperaturerefluxed for 1 h
  2. temperatureAfter refluxing o.n
  3. concentrationwas concentrated in vacuo to about ½ of its volume
  4. customresulting in a precipitate which
  5. filtrationwas filtered off
  6. customrecrystallized from EA/Hep