HRID2425329

反应详情

EQUATION

反应方程式

HRID 2425329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

6-Bromoindole-3-carboxaldehyde, 23 (5.0 g, 22.3 mmol) is dissolved in methylene chloride (40 mL), then cooled to 0° C. and tert-butylchloroformate (3.40 g, 25.0 mmol) and triethyl amine (2.50 g, 25.0 mmol) are added over 5 minutes. The reaction is maintained at reflux, under inert atmosphere for 3 hours. The reaction is cooled, filtered and the solvent removed in vacuo. The residue composed primarily of compound 24 is used in the Example 18 without purification. (See, e.g., G. Wille and W. Steglich, Synthesis, 2001, 759-762 for a related procedure.)

WORKUP

后处理

  1. temperatureThe reaction is maintained
  2. temperatureat reflux, under inert atmosphere for 3 hours
  3. temperatureThe reaction is cooled
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customis used in the Example 18 without purification
  7. customSteglich, Synthesis, 2001, 759-762 for a related procedure