HRID551085

反应详情

EQUATION

反应方程式

HRID 551085 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (±)-2a-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-2a,5-dihydropyrrolo[4,3,2-de]quinoline-2,4(1H,3H)-dione from Step A (2.30 g, 6.62 mmol) and hydrazine (1.05 mL, 33.1 mmol) in EtOH (30 mL) was heated at 70° C. for 2 h, then cooled to ambient temperature and filtered. The filtrate was concentrated in vacuo. The crude product was purified by silica gel chromatography, eluting with a gradient of CH2Cl2:MeOH:NH4OH—100:0:0 to 90:9:1, to give the title compound. MS: m/z=218 (M+1).

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated in vacuo
  3. customThe crude product was purified by silica gel chromatography
  4. washeluting with a gradient of CH2Cl2