HRID1598477

反应详情

EQUATION

反应方程式

HRID 1598477 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-benzyl 2(R)-tert-butoxycarbonylaminohexanamide (1.0 g, 2.29 mmol) in THF (10 mL) was vigorously stirred with 6N HCl(10 mL) for 24h. Ethyl acetate was added, and the layers separated. The organic phase was washed with water, then saturated sodium chloride solution. The crude product was chromatographed on silica gel with 30% ethyl acetate in hexane. The title compound was obtained as an oil (0.140 g). NMR (CDCl3, 300 MHz) δ 7.3 (5H, m), 6.31, 6.14 (1H, 2 ds, J=7, 7 Hz), 5.55, 5.42 (1H, 2 ds, J=7, 7 Hz), 4.68 (2H, AB q, J=15 Hz, D n=36 Hz), 4.78 (1H, m), 1.66 (2H, m), 1.47 (9H, d), 1.33 (4H, m), 0.89 (3H, brt, J=7 Hz).

WORKUP

后处理

  1. customthe layers separated
  2. washThe organic phase was washed with water
  3. customThe crude product was chromatographed on silica gel with 30% ethyl acetate in hexane