HRID1612775

反应详情

EQUATION

反应方程式

HRID 1612775 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 13.44 g of methallylamine hydrochloride and 27.3 g of di-tert.-butyl carbonate in 250 ml of dichloromethane at 20° is treated with 25.2 g of triethylamine. The solution is stirred for 1 hour at 20° washed with water and the organic phase is dried and the solvent is removed to give a colourless oil. Flash-chromatography on silica-gel affords pure 3-(N-tert.-butoxycarbonylamino)-2-methyl-prop-2-ene as a colourless oil; 1H-NMR (CDCl3): δ (ppm)=4.83 (2H, m, 2×CH=C), 4.70-4.60 (1H, broad s, exch. D2O, NH), 3.67 (2H, s, CH2N), 1.73 (3H, s, CH3), 1.45 (9H, s, tBu).

WORKUP

后处理

  1. washwashed with water
  2. customthe organic phase is dried
  3. customthe solvent is removed
  4. customto give a colourless oil