HRID518485

反应详情

EQUATION

反应方程式

HRID 518485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of 7-methoxyfuro[2,3-c]pyridine (2.9 g, 19.6 mmol) in THF (20 mL) stirred under an atmosphere of argon was added n-BuLi (7.8 mL, 19.6 mmol) at −78° C.; the mixture was transferred to a −30° C. ice bath and was stirred for 2 h. The mixture was cooled to −78° C. and MeI (4.2 g, 29.4 mmol) was added. After the mixture was stirred at rt for 18 h, the reaction mixture was quenched with water (30 mL) and extracted with DCM (50 mL×3). The combined organic layers were washed with brine (30 mL×3), dried over Na2SO4 and concentrated in vacuo to afford the title compound (3.2 g, 100%) as a yellow solid. The material was carried forward without any further purification. LCMS (M+H)+=164.

WORKUP

后处理

  1. customwas transferred to a −30° C.
  2. stirringAfter the mixture was stirred at rt for 18 h
  3. customthe reaction mixture was quenched with water (30 mL)
  4. extractionextracted with DCM (50 mL×3)
  5. washThe combined organic layers were washed with brine (30 mL×3)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo