HRID335795

反应详情

EQUATION

反应方程式

HRID 335795 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 5-bromo-2-(6-chloro-2-fluoropyridin-3-yloxy)-N,N-diethylbenzamide (120 mg, 0.299 mmol) in 5 mL of dry THF at −78 C was added dropwise lithium diisopropylamide, 2.0 m heptane/tetrahydrofuran/ethylbenzene (158 μL, 1.195 mmol) (0.6 mL of 2M solution) and the reaction was stirred at −78 C for 3 h. The reaction was quenched at −78 C with sat. NH4Cl and was allowed to warm up to RT. The reaction was extracted with EA, dried over Na2SO4, filtered and evaporated to dryness. CC (hexane to H/DCM=1:1 to DCM) gave 7-bromo-3-chloro-1-fluoro-5H-chromeno[2,3-c]pyridin-5-one as an offwhite solid. MS (M+1): 328.

WORKUP

后处理

  1. customThe reaction was quenched at −78 C with sat. NH4Cl
  2. extractionThe reaction was extracted with EA
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness