HRID1622316

反应详情

EQUATION

反应方程式

HRID 1622316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-(3-cyanophenyl)-1H-naphtho[1,2-b][1,4]diazepin-2,4(3H,5H)-dione (37 mg, 0.11 mmol), hydroxylamine hydrochloride (76 mg, 1.1 mmol) and triethylamine (0.16 mL, 1.1 mmol) in THF (0.65 mL)/methanol (1.3 mL) was heated under reflux for 2 hours. The solvent was removed under reduced pressure, and to the residue was added water (4 mL). The precipitated crystal was filtered and washed with water. The crystal was dried in vacuo at 50° C., to give the titled compound as a light gray crystal (36 mg, 91%).

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. customThe solvent was removed under reduced pressure
  3. additionto the residue was added water (4 mL)
  4. filtrationThe precipitated crystal was filtered
  5. washwashed with water
  6. customThe crystal was dried in vacuo at 50° C.