HRID1721533

反应详情

EQUATION

反应方程式

HRID 1721533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

N-Methylephedrine (500 mg, 2.79 mmol) was added to a solution of o-iodobenzoic acid I (7.8 g; 27.9 mmol) in DMSO (55 ml). After 48 hours the solution was diluted with NaHCO3 (2.5%, 30 ml) and extracted with ethyl acetate (3×10 ml). The combined organic layers were washed with water (2×5 ml), dried over sodium sulfate and evaporated to dryness under vacuum. The residue was purified by distillation to give 460 mg (92%) of 2-dimethylamino-1-phenyl-propan-1-one (boiling at 113°-117° C./12 mm).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×10 ml)
  2. washThe combined organic layers were washed with water (2×5 ml)
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness under vacuum
  5. distillationThe residue was purified by distillation