HRID260192

反应详情

EQUATION

反应方程式

HRID 260192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.63 g (5 mmol) of the product of Example 26 in 10 ml of acetone, 1.41 g (10 mmol) methyl iodide were added and the mixture was refluxed overnight while stirring. The acetone layer was separated by decantation and the yellowish, oily residue was crystallized from methanol/ether. Yield, 1.94 g (83%), m.p. 155°-157° C. PMR (D2O) δ 9.16-8.00 (m, 4H, C5H4N+), 7.33-6.83 (m, 4H, C6H4), 4.40 (s, 3H, N+ --CH3), 3.5 (t, 2H, J=7 Hz, ##STR1455## 2.90 (t, 2H, J=7 Hz, CH2), 1.30 (s, 9H, C--(CH3)3). Anal. (C20H25N2O3I) C, H, N.

WORKUP

后处理

  1. temperaturethe mixture was refluxed overnight
  2. customThe acetone layer was separated by decantation
  3. customthe yellowish, oily residue was crystallized from methanol/ether
  4. customYield