HRID4202

反应详情

EQUATION

反应方程式

HRID 4202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-diisopropylaminoethyl chloride hydrochloride (40.0 g, 0.2 mole) and potassium phthalimide (74.0 g, 0.4 mole) as stirred overnight at 85° C. in 500 ml of dimethyl formamide. The reaction mixture was stirred to dryness on a rotary evaporator, and the residue was partitioned between chloroform and water. The chloroform layer was extracted with 10% sodium hydroxide. After drying and removal of solvent, a brown oil was obtained which slowly crystallized. A portion of the oil was converted to the hydrochloride salt and recrystallized from methanol/diethyl ether to give 4.18 g (62.3%) of white crystalline product, m.p. 209°-211° C.

WORKUP

后处理

  1. customthe residue was partitioned between chloroform and water
  2. extractionThe chloroform layer was extracted with 10% sodium hydroxide
  3. customAfter drying
  4. customremoval of solvent
  5. customa brown oil was obtained which
  6. customslowly crystallized
  7. customrecrystallized from methanol/diethyl ether