反应详情

To an ice water cooled stirred suspension of 1.3 g of 6-(methylthio)-benz[cd]indol-2(1H)-one (Example 2) in 25 ml of ethanol is added portionwise over 12 minutes 1.2 g of 85% m-chloroperbenzoic acid at a rate so the temperature is kept below 7° C. Stirring is continued over 1.25 hours. The reaction mixture is poured over crushed ice and 8 ml of 1N sodium hydroxide with stirring. After 15 minutes of additional stirring, the reaction mixture is filtered. The filtrate is extracted with methylene chloride, dried with magnesium sulfate and evaporated to afford 0.65 g of the desired product as a yellow solid, m.p. 178°-185° C.

1. customis kept below 7° C
2. stirringStirring
3. additionThe reaction mixture is poured
4. stirringwith stirring
5. waitAfter 15 minutes of additional stirring
6. filtrationthe reaction mixture is filtered
7. extractionThe filtrate is extracted with methylene chloride
8. dry with materialdried with magnesium sulfate
9. customevaporated