HRID53557

反应详情

EQUATION

反应方程式

HRID 53557 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-acetyl-2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (3.36 g) in acetonitrile (20 mL) cooled on ice was added nitronium tetrafluoroborate (85%, 2.26 g). The mixture was removed from the ice bath and was stirred for 5 hours. The reaction then was quenched with 10% potassium carbonate. Ethyl acetate was added and the organic phase was separated, washed, dried, and evaporated. Chromatography over silica gel gave 0.71 g of the title compound, which crystallized from diisopropyl ether, m.p. 140-141.

WORKUP

后处理

  1. customThe mixture was removed from the ice bath
  2. customThe reaction
  3. customthen was quenched with 10% potassium carbonate
  4. additionEthyl acetate was added
  5. customthe organic phase was separated
  6. washwashed
  7. customdried
  8. customevaporated