HRID78108

反应详情

EQUATION

反应方程式

HRID 78108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 2-(2-nitro-ethyl)-5-phenoxy-pyridine (76 mg, 0.31 mmol) described in Manufacturing Example 121-1-4 and methanol (6.0 mL) was added lithium methoxide (24 mg, 0.62 mmol) at room temperature, which was stirred for 3 minutes, and then the solvent was evaporated under a reduced pressure. Methylene chloride (10 mL) was added to the residue, titanium(IV) chloride (0.11 mL, 1.0 mmol) was added at room temperature, which was stirred for 10 minutes. Cold aqueous sodium bicarbonate and ethyl acetate were added to the reaction solution, which was filtered through a Celite pad, and then the organic layer was separated. The organic layer was concentrated under a reduced pressure to obtain the title compound (56 mg, 69%).

WORKUP

后处理

  1. customthe solvent was evaporated under a reduced pressure
  2. additionwas added at room temperature
  3. stirringwhich was stirred for 10 minutes
  4. filtrationwas filtered through a Celite pad
  5. customthe organic layer was separated
  6. concentrationThe organic layer was concentrated under a reduced pressure