HRID2096246
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
2-[2-(Tritylsulfanyl)benzyl]-1H-isoindole-1,3(2H)-dione (4.7 g, 9.19 mmol) was suspended in EtOH (150 mL) and treated with hydrazine monohydrate 65% (4.66 mL, 62 mmol). The mixture was heated under reflux for 1.5 h, cooled to RT and the precipitate was filtered. The filtrate was concentrated, triturated with EtOAc and filtered. The filtrate was concentrated under reduced pressure to afford the title compound (3.0 g, 86%) as a colourless oil. 1H NMR (300 MHz, CDCl3): δ 7.34-7.28 (6H, m), 7.26-7.18 (9H, m), 7.15 (2H, m), 7.10 (1H, m), 6.93-6.85 (1H, m), 3.40 (2H, s).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 1.5 h
- filtrationthe precipitate was filtered
- concentrationThe filtrate was concentrated
- customtriturated with EtOAc
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure