HRID1783953

反应详情

EQUATION

反应方程式

HRID 1783953 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

A solution of 1-trifluoroacetyl-4-(4-nitrophenyl)piperidine (1.42 g, 4.7 mmol) in THF (15 mL) is stirred in 25 mL 2-necked flask fitted with a condenser and pressure-equalizing addition funnel. The system is flushed with N2, NaBH4 (210 mg, 5.6 mmol) is added and the flask is cooled to 0° C. A solution of iodine (600 mg, 2.3 mmol) in THF (5 mL) is then added dropwise over 20 minutes, after which the addition funnel is removed and the mixture heated at reflux overnight. The resulting pale yellow suspension is cooled to rt and MeOH (1.5 mL) is added cautiously, causing vigorous evolution of a gas. Evaporation of the solvents affords the title compound, which is used without further purification.

WORKUP

后处理

  1. customfitted with a condenser and pressure-equalizing addition funnel
  2. additionis added
  3. customafter which the addition funnel is removed
  4. temperaturethe mixture heated
  5. temperatureat reflux overnight
  6. temperatureThe resulting pale yellow suspension is cooled to rt
  7. additionMeOH (1.5 mL) is added cautiously
  8. customEvaporation of the solvents