HRID2098011

反应详情

EQUATION

反应方程式

HRID 2098011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

CuCN (0.211 g, 2.36 mmol) and Pd(PPh3)4 (0.136 g, 0.118 mmol) were added to a solution of methyl 2-(7-bromo-2-oxoquinolin-1(2H)-yl)acetate (0.35 g, 1.18 mmol) in DMF (1 mL) in a screw cap vial. The vial was sealed and placed into a oil bath at 120° C. and the reaction mixture was stirred for 18 h. The resulting mixture was diluted with Et2O and washed with brine. The organic phase was separated, dried (Na2SO4), filtered, concentrated under vacuum and the residue was purified on a silica gel column to give methyl 2-(7-cyano-2-oxoquinolin-1(2H)-yl)acetate (0.204 g, 71%). Retention time (min)=1.464, method [1], MS (ESI) 243.1 (M+H).

WORKUP

后处理

  1. customcap vial
  2. customThe vial was sealed
  3. customplaced into a oil bath at 120° C.
  4. washwashed with brine
  5. customThe organic phase was separated
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum
  9. customthe residue was purified on a silica gel column