HRID850765
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
10-bromo-2-hydroxy-4H-pyrido[3,2,1-jk]carbazole-4-one (2.5 g) obtained in Example 59 was suspended in dimethyl sulfoxide (120 ml), and potassium carbonate (2.2 g) was added to the suspension. The mixture was stirred at room temperature for 30 minutes and t-butyl bromoacetate (1.4 ml) was added to the mixture. The mixture was stirred at room temperature for 12 hours, and the reaction mixture was poured into ice water (900 ml), and the crystals precipitated were recovered by filtration. The crude crystals were purified by silica gel flash column chromatography (eluent: methylene chloride containing 2% methanol) to obtain the title compound (1.9 g, 68%).
WORKUP
后处理
- stirringThe mixture was stirred at room temperature for 12 hours
- customthe crystals precipitated
- filtrationwere recovered by filtration
- customThe crude crystals were purified by silica gel flash column chromatography (eluent: methylene chloride containing 2% methanol)