HRID532935

反应详情

EQUATION

反应方程式

HRID 532935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

100-3. NH2OH*HCl (51 mg, 0.74 mmol) was added to a mixture of (E)-9-(3-(dimethylamino)acryloyl)-3,4,7,8-tetrahydro-[1,4]diazepino[7,1-a]isoquinoline-2,5-dione (160 mg, 0.49 mmol) in MeOH (5 mL) and the solution was heated to reflux for 1 h. The mixture was then concentrated in vacuo and the crude product was purified by flash chromatography (SiO2, DCM/MeOH 99:1 to 90:10) to afford the title compound (90 mg) as a beige solid. UPLC-MS: MS 296.1 (M-FH+). UPLC rt 0.65 nm.

WORKUP

后处理

  1. temperaturethe solution was heated
  2. temperatureto reflux for 1 h
  3. concentrationThe mixture was then concentrated in vacuo
  4. customthe crude product was purified by flash chromatography (SiO2, DCM/MeOH 99:1 to 90:10)