HRID1435952

反应详情

EQUATION

反应方程式

HRID 1435952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1 g (4.29 mmol) of N-(tert-butoxycarbonyl)-DL-aspartic acid and 0.98 g (5.15 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI) in 100 mL of DCM, was stirred at room temperature overnight. The solution was extracted three times with 5% aq. NaHSO4, the organic extracts were dried over anh. sodium sulfate and the solvent evaporated under vacuum. In this way 750 mg of the title compound were recovered. 1H NMR (400 MHz, DMSO-D6) δ ppm 1.38 (s, 9 H) 2.78-2.90 (m, 1 H) 3.15-3.28 (m, 1 H) 4.54-4.65 (m, 1 H) 7.73 (d, J=7.91 Hz, 1 H).

WORKUP

后处理

  1. extractionThe solution was extracted three times with 5% aq. NaHSO4
  2. dry with materialthe organic extracts were dried over anh. sodium sulfate
  3. customthe solvent evaporated under vacuum
  4. customIn this way 750 mg of the title compound were recovered