HRID523552

反应详情

EQUATION

反应方程式

HRID 523552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Polyphosphoric acid (7 g) was added to a solution of 1-(4-bromo-phenylsulfanyl)-propan-2-one (I-24a: 2.0 g, 8.163 mmol) in toluene (10 mL) and the resulting mixture was heated to 100° C. for 5 hours. The reaction was monitored by TLC (100% hexane). The reaction mixture was cooled to room temperature, quenched with ice, basified with potassium carbonate (pH˜8) and extracted with ethyl acetate. The organic layer was concentrated to yield the crude product. Purification by column chromatography on silica gel (100% hexane) afforded 1.2 g of product (66% yield)

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customquenched with ice
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic layer was concentrated
  5. customto yield the crude product
  6. customPurification by column chromatography on silica gel (100% hexane)