HRID34743

反应详情

EQUATION

反应方程式

HRID 34743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Amino-3-methyl-2-butanone hydrochloride hydrate [J. Org. Chem. 49, 1209 (1984)] (10.6 g., 0.076 mol was dissolved in 700 ml. 1:1 THF:H2O and the pH adjusted to 6.8 with dilute NaOH. Benzylchloroformate (11.93 ml., 0.084 ml.) was added dropwise, maintaining pH 6.8-7.0 by the simultaneous dropwise addition of dilute NaOH. The pH was so maintained until it stabilized. The reaction mixture was extracted 4×100 ml. CHCl3. The organic extracts were combined, filtered and stripped to yield title product as an oil, 9.26.

WORKUP

后处理

  1. dissolution, 0.076 mol was dissolved in 700 ml
  2. temperaturemaintaining pH 6.8-7.0
  3. temperatureThe pH was so maintained until it
  4. extractionThe reaction mixture was extracted 4×100 ml
  5. filtrationfiltered