HRID1484410

反应详情

EQUATION

反应方程式

HRID 1484410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the stirred solution of (5-Bromo-pyridin-2-yl)-Methanol (5 gm, 26.59 mmol, 1 eq) in DCM (50 mL) at 0° C. is added Thionyl chloride (3 mL) drop wise at RT then stirred at RT for 4 h. After completion, the reaction mixture quenched with saturated sodium bicarbonate solution and extracted with DCM (3×100 mL). The combined organic layer dried over sodium sulphate and evaporated under reduced pressure. The crude is purified by column chromatography using silica 100-200 mesh using 10% EtOAc: Hexane as eluent to afford title compound (4 g) as brown colored liquid. 1NMR (400 MHz, DMSO) δ: 4.77 (s, 2H), 7.54 (d, J=8.64 Hz, 1H), 8.09-8.12 (dd, J1=2.4 Hz, J2=8.32 Hz, 1H), 8.70 (d, J=5.96 Hz, 1H).

WORKUP

后处理

  1. customAfter completion, the reaction mixture quenched with saturated sodium bicarbonate solution
  2. extractionextracted with DCM (3×100 mL)
  3. dry with materialThe combined organic layer dried over sodium sulphate
  4. customevaporated under reduced pressure
  5. customThe crude is purified by column chromatography