HRID648509

反应详情

EQUATION

反应方程式

HRID 648509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium borohydride (0.058 g) was added to a solution of 1-(4-aminobenzoyl)-4-(4-fluorobenzoyl)piperidine (1.0 g) in methanol (80 ml) and the mixture was stirred at room temperature for 2 hours. Additional sodium borohydride (0.050 g) was added. After being stirred at the same temperature for 1.5 hours, the resultant mixture was concentrated in vacuo. The residue was diluted with water and extracted twice with methylene chloride. The extracts were combined, washed with brine, dried over magnesium sulfate, and concentrated to dryness in vacuo. The powdery residue was washed with diisopropyl ether to give 1-(4-aminobenzoyl)-4-[(4-fluorophenyl)hydroxymethyl]piperidine (1.00 g) as pale yellow powder.

WORKUP

后处理

  1. stirringAfter being stirred at the same temperature for 1.5 hours
  2. concentrationthe resultant mixture was concentrated in vacuo
  3. additionThe residue was diluted with water
  4. extractionextracted twice with methylene chloride
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated to dryness in vacuo
  8. washThe powdery residue was washed with diisopropyl ether