HRID1085174
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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, ##STR1473## 7.33-6.83 (m 4H, C6H4), 4.40 (s, 3H, N--CH3), 3.5 (t, 2H, J=7 Hz, ##STR1474## 2.90 (t, 2H, J=7 Hz, CH2), 1.30 (s, 9H, C--CH3)3). Anal. (C20H25N2O3I) C, H, N.
WORKUP
后处理
- temperaturethe mixture was refluxed overnight
- customThe acetone layer was separated by decantation
- customthe yellowish, oily residue was crystallized from methanol/ether
- customYield