HRID2102297
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturerefluxed for 1 h
- temperatureAfter refluxing o.n
- concentrationwas concentrated in vacuo to about ½ of its volume
- customresulting in a precipitate which
- filtrationwas filtered off
- customrecrystallized from EA/Hep