HRID1436750

反应详情

EQUATION

反应方程式

HRID 1436750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (1R,4S)-4-[(tert-butoxycarbonyl)amino]cyclopent-2-ene-1 -carboxylic acid (10.0 g, 44 mmol) in DMF (25 mL) was added potassium carbonate (6.33 g, 45.8 mmol) followed by methyl iodide (4.0 mL, 64 mmol). After being stirred at room temperature overnight, the reaction mixture was diluted with EtOAc. The solution was washed with water four times and brine one time, dried (MgSO4) and concentrated. The residue was dried under high vacuum overnight to provide the title compound (11 g, 99%). MS calculated for C12H19NO4:(M+H)+242; found 142.1 (M-Boc+H)+. 1H NMR (CDCl3) δ 5.86 (m, 2H), 4.90 (m, 1H), 4.80 (m, 1H), 3.72 (s, 3H), 3.50 (m, 1H), 2.51 (m, 1H), 1.86 (m, 1H), 1.42 (s, 9H).

WORKUP

后处理

  1. washThe solution was washed with water four times and brine one time
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customThe residue was dried under high vacuum overnight