HRID2259285

反应详情

EQUATION

反应方程式

HRID 2259285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,5-Dimethylbenzyl 2-(1,1-dimethylethoxycarbonylamino)-3-(3-indolyl)propionate (1.0 g) was dissolved in dry tetrahydrofuran (20 ml). Saturated methanolic hydrochloric acid (10 ml) was added and the reaction was stirred for 16 hours. The solvent was removed in vacuo and the residue was recrystallised from ethanol/diethyl ether to yield 3,5-dimethylbenzyl 2-amino-3-(3-indolyl)propionate hydrochloride (0.71 g), m.p. 213°-214° C. 1H NMR (360 MHz D6DMSO) δ11.09 (1H, s), 8.64 (1H, s), 7.51 (1H, d, J=7 Hz), 7.38 (1H, d, J=7 Hz), 7.20 (1H, d, J=2 Hz), 7.10 (1H, t, J=7 Hz), 6.98 (1H, t, J=7 Hz), 6.94 (1H, s), 6.76 (2H, s). Found: C, 66.25; H, 6.67; N, 7.71, C20H22N2O2. HCl. 0.25(H2O) requires C, 66.11; H, 6.52; N, 7.71%.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customthe residue was recrystallised from ethanol/diethyl ether