반응 #1865

반응 방정식

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

potassium carbonate

dimethylsulfate

→

oil

수율 86.2%

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

수율 86.2%

용매

acetone

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   기타The addition funnel was replaced with a condenser
3. 3
   온도the slurry was refluxed for 18 hours
4. 4
   여과The K2CO3 was filtered off
5. 5
   세척washed well with acetone
6. 6
   기타Acetone was evaporated
7. 7
   기타the residue was purified by column chromatography

실험 절차

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.

출처