HRID381694

反应详情

EQUATION

反应方程式

HRID 381694 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 140 g of N-carbamylmaleimide (1 mole), 1.36 g of zinc chloride (0.01 moles) and 150 g of n-butanol (2 moles) was heated to reflux. After 4 hours, the mixture was poured into 400 mL of water and cooled to room temperature. The butyl maleurate was filtered, washed with water and dried to afford 200 g (93% yield). M.P.: 97°-90° C.; 1H NMR (CDCl3): δ10.6 (brs, 1H), 8.2 (brs, 1H), 6.3 (AB, 2H), 5.9 (brs, 1H), 4.2 (t, 2H), 1.6 (m, 2H), 1.4 (m, 2H), 0.9 (t, 3H); HPLC (20 to 40% CH3CN/H2O over 20 minutes, C8): Rt=9.4 minutes.

WORKUP

后处理

  1. temperaturewas heated to reflux
  2. filtrationThe butyl maleurate was filtered
  3. washwashed with water
  4. customdried
  5. customto afford 200 g (93% yield)