HRID13553

反应详情

EQUATION

反应方程式

HRID 13553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of cyclohexanecarboxaldehyde bisulfite adduct (5.0 mmol) and Et3 N (5.5 mmol) in dichloroethane (20 mL) was stirred at room temperature for 15 min. The suspension was treated with N-methylbenzylamine (5.5 mmol) and was stirred for 45 min. NaBH(OAc)3 (7.0 mmol) was added portion-wise over approximately 30 min. After 16 h, the reaction mixture was diluted with EtOAc (80 mL), and was washed with 1 N NaOH (25 mL) followed by brine (25 mL). The organic layer was dried (MgSO4) and concentrated to yield benzyl-cyclohexylmethyl-methyl-amine as an oil. The crude material was purified by the General Purification Method as described above.

WORKUP

后处理

  1. stirringwas stirred for 45 min
  2. waitAfter 16 h
  3. washwas washed with 1 N NaOH (25 mL)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. concentrationconcentrated