HRID34745

反应详情

EQUATION

反应方程式

HRID 34745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Bromoquinoline (3.29 ml., 0.032 mol) was dissolved in 300 ml. THF and cooled to -78°. n-Butyllithium (13.6 ml. of 2.5M in hexane, 0.034 ml.) was added slowly and the mixture stirred 15 minutes at -75° to -78°. N-(Dimethoxyacetyl)morpholine (5.98 g., 0.032 mol) in 10 ml. THF was then added and stirring continued for 1.75 hours at the same temperature. The reaction was then quenched into 300 ml. saturated NH4Cl. The aqueous layer was separated and extracted 4×100 ml. ether. The organic layers were combined, dried over MgSO4, stripped to yield title product, 7.0 g., bp 120°-123°/0.125 torr.

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 1.75 hours at the same temperature
  3. customThe reaction was then quenched into 300 ml
  4. customThe aqueous layer was separated
  5. extractionextracted 4×100 ml
  6. dry with materialdried over MgSO4