HRID1035229

反应详情

EQUATION

反应方程式

HRID 1035229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Intermediate 60A (3.48 g, 9.47 mmol) was dissolved in dichloromethane (150 mL) and the mixture was cooled in an ice bath. While stirring, thionyl chloride (0.76 mL, 10.4 mmol) was added dropwise. The cooling bath was removed after 30 min. The mixture was stirred for 2.5 h and then evaporated to dryness. The residue was purified by column chromatography eluting with dichloromethane. There was obtained 2.93 g (80%) of 60B as a solid. 1H NMR (500 MHz, CDCl3): δ 4.22 (m, 2H), 4.57 (s, 2H), 4.65 (m, 2H), 5.14 (m, 1H), 7.29 (d, 2H), 7.36 (d, 2H), 7.53 (t, 2H), 7.59 (t, 1H), 8.16 (d, 2H), MS (APCI+) m/z 386 [M+H]+.

WORKUP

后处理

  1. temperaturethe mixture was cooled in an ice bath
  2. customThe cooling bath was removed after 30 min
  3. stirringThe mixture was stirred for 2.5 h
  4. customevaporated to dryness
  5. customThe residue was purified by column chromatography
  6. washeluting with dichloromethane