HRID551085
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
- customThe crude product was purified by silica gel chromatography
- washeluting with a gradient of CH2Cl2