HRID1046410

反应详情

EQUATION

反应方程式

HRID 1046410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 2-chloro-pyridine-4-carbaldehyde and (300 mg, 2.12 mmol) and pyrrolidine (0.19 mL, 2.12 mmol) in DCM (10 mL) was treated with acetic acid (0.25 mL, 4.24 mmol). The mixture was stirred at room temperature for 10 minutes and NaBH(OAc)3 (899 mg, 4.24 mmol) was added. After overnight stirring, the reaction was washed with sat. NaHCO3 and extracted twice with DCM. The organic layers were combined and washed with water, brine, dried over sodium sulfate, filtrated and concentrated. The crude material was purified by column chromatography with MeOH/DCM (0-10%) and concentrated to give 120 mg of 2-chloro-4-pyrrolidin-1-ylmethyl-pyridine as a clear oil.

WORKUP

后处理

  1. stirringAfter overnight stirring
  2. washthe reaction was washed with sat. NaHCO3
  3. extractionextracted twice with DCM
  4. washwashed with water, brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltrated
  7. concentrationconcentrated
  8. customThe crude material was purified by column chromatography with MeOH/DCM (0-10%)
  9. concentrationconcentrated