HRID263715

反应详情

EQUATION

反应方程式

HRID 263715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.93 g (50 mmol) of t-butyl 2-aminoacetate was dissolved in 65 ml of benzene. To the above mixture, 4.41 g (52.5 mmol) of diketene was added dropwise and the reaction mixture was stirred for one hour. The reaction mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate and then with water, and dried over anhydrous sodium sulfate. The solvent was distilled away from the reaction mixture under reduced pressure, whereby 9.821 g (91.2%) of the captioned compound was obtained. NMR (δ, CDCl3) 1.47 (9H, s), 2.28 (3H, s), 3.46 (2H, s), 3.96 (2H, d, J=5 Hz), 7.33 (1H, s)

WORKUP

后处理

  1. washThe reaction mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate
  2. dry with materialwith water, and dried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled away from the reaction mixture under reduced pressure