HRID473022

反应详情

EQUATION

反应方程式

HRID 473022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of compound 6 (40 mg, 0.11 mmol) in DCM (3 mL) was added TiCl4 (0.22 mL, 0.22 mmol) and the mixture was stirred in microwave at 50° C. for 10 min. After the reaction, bis-trimehtlysilylcarbodiimide (62 mg, 0.33 mmol) was added and the mixture was stirred in microwave at 60° C. for 10 min. The reaction was quenched with ice water and extracted with CH2Cl2, the organic layer was washed with water, brine, dried and concentrated to give the product 7 (20 mg, 57%).

WORKUP

后处理

  1. customAfter the reaction, bis-trimehtlysilylcarbodiimide (62 mg, 0.33 mmol)
  2. additionwas added
  3. stirringthe mixture was stirred in microwave at 60° C. for 10 min
  4. customThe reaction was quenched with ice water
  5. extractionextracted with CH2Cl2
  6. washthe organic layer was washed with water, brine
  7. customdried
  8. concentrationconcentrated