HRID606051

反应详情

EQUATION

反应方程式

HRID 606051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

An aqueous solution (125 mL) of sodium dithionate (38.0 g, 218 mmol) was added to a solution of 2-chloro-3-nitro-N-pent-4-ynylquinolin-4-amine (12.64 g, 43.63 mmol) in ethanol (15 mL) and acetonitrile (130 mL). A fine white precipitate formed within seconds. After 2.5 hours, the volatiles were removed under reduced pressure leaving a yellow aqueous mixture that was diluted with water (1 L) and washed with dichloromethane (250 mL×3). The organic layers were combined, washed with water and brine, dried over magnesium sulfate, filtered, and concentrated to yield 2-chloro-N4-pent-4-ynylquinoline-3,4-diamine as an amber oil (8.10 g) that was used without further purification.

WORKUP

后处理

  1. customA fine white precipitate formed within seconds
  2. customthe volatiles were removed under reduced pressure
  3. customleaving a yellow aqueous mixture that
  4. washwashed with dichloromethane (250 mL×3)
  5. washwashed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated