HRID2234222

反应详情

EQUATION

反应方程式

HRID 2234222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (6-chloro-5-methoxypyridin-3-yl)methanol (0.50 g, 2.9 mmol) in dichloromethane (14 mL) at 25° C. was added thionyl chloride (230 μL, 3.2 mmol) dropwise. Let stir for 5 h, then the reaction was quenched with saturated aqueous NaHCO3 and extracted with dichloromethane (3×). The combined organic layer were dried over MgSO4 and concentrated to furnish the product 2-chloro-5-chloromethyl-3-methoxypyridine that was 96% pure by GC-MS. The product was used immediately in the next step without further purification. GC-MS: Exact mass calcd for C7H7Cl2NO [M]+, 191. Found 191.

WORKUP

后处理

  1. customthe reaction was quenched with saturated aqueous NaHCO3
  2. extractionextracted with dichloromethane (3×)
  3. dry with materialThe combined organic layer were dried over MgSO4
  4. concentrationconcentrated