反応 #4471

反応方程式

product

6-Fluoro-1,2,3,9-tetrahydro-4H-carbazol-4-one

potassium carbonate

dimethylsulphate

→

title compound

収率 97.5%

6-Fluoro-1,2,3,9-tetrahydro-9-methyl-4H-carbazol-4-one

収率 97.5%

溶媒

acetone

反応条件

後処理

1. 1
   濃縮The mixture was concentrated to one half of its volume
2. 2
   ろ過The mixture was filtered off
3. 3
   洗浄washed with water (50 ml)
4. 4
   その他air-dried for 1 h
5. 5
   乾燥dried in vacuo over phosphorus pentoxide

実験手順

The product of Stage (ii) (7.28 g), potassium carbonate (9.90 g), acetone (70 ml), and dimethylsulphate (5.1 ml) were vigorously stirred at room temperature overnight under nitrogen. The mixture was concentrated to one half of its volume and then stirred with water (350 ml) for 30 min. The mixture was filtered off, washed with water (50 ml), air-dried for 1 h, and dried in vacuo over phosphorus pentoxide to give the title compound as needles (7.59 g), m.p. 157.5°-158.5°.

出典