反应 #344377

反应方程式

1,3-dihydro-4-hydroxy-1,3-dimethyl-2H-indol-2-one

potassium carbonate

dimethylsulfate

→

oil

收率 86.2%

1,3-Dihydro-4-methoxy-1,3-dimethyl-2H-indol-2-one

收率 86.2%

溶剂

acetone

反应条件

后处理

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   其他The addition funnel was replaced with a condenser
3. 3
   温度the slurry was refluxed for 18 hours
4. 4
   过滤The K2CO3 was filtered off
5. 5
   洗涤washed well with acetone
6. 6
   其他Acetone was evaporated
7. 7
   其他the residue was purified by column chromatography

实验过程

A slurry of 1,3-dihydro-4-hydroxy-1,3-dimethyl-2H-indol-2-one (50 g), milled potassium carbonate (60.1 g) and HPLC grade acetone (400 ml) was mechanically stirred at room temperature as dimethylsulfate (41.4 ml) was added dropwise. The addition funnel was replaced with a condenser and the slurry was refluxed for 18 hours. The K2CO3 was filtered off and washed well with acetone. Acetone was evaporated and the residue was purified by column chromatography to yield 46.5 g of an oil. The oil was dissolved in ether and placed in the refrigerator where, upon standing overnight, the product crystallized, m.p. 73°-74° C.

来源