反応式
[CH2:1]([C:3]1[S:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[CH:4]=1)[CH3:2].[C:12](Cl)(=[O:14])[CH3:13].Cl>ClC(Cl)C>[CH2:1]([C:3]1[S:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[C:4]=1[C:12](=[O:14])[CH3:13])[CH3:2]参加物
実験手順
Into a one-litre flask fitted with a mechanical stirrer and a dropping-funnel, 32.45 g (0.2 mol) of 2-ethyl-benzo[b]thiophene and 14.3 ml of acetyl chloride were introduced with 400 ml of dichloroethane. After the solution was cooled to between 5 and 10° C by means of an ice-bath, 23.2 ml (0.2 mol) of stannic chloride were introduced through the dropping-funnel. The mixture was then allowed to return to room temperature and was stirred for about 14 hours. The complex so formed was then hydrolysed with diluted hydrochloric acid. The organic and aqueous phases were separated by decantation and the aqueous phase was extracted with ether. The ethereal fraction was then added to the organic phase and the mixture was washed with water and evaporated to dryness to give, after distillation between 124°-134° C (0.01 mm/Hg), 31.3 g of 2-ethyl-3-acetyl-benzo[b]thiophene. Yield 765%.
後処理
- customInto a one-litre flask fitted with a mechanical stirrer and a dropping-funnel
- temperatureAfter the solution was cooled to between 5 and 10° C by means of an ice-bath
- customto return to room temperature
- customThe complex so formed
- customThe organic and aqueous phases were separated by decantation
- extractionthe aqueous phase was extracted with ether
- additionThe ethereal fraction was then added to the organic phase
- washthe mixture was washed with water
- customevaporated to dryness
- customto give
- distillationafter distillation between 124°-134° C (0.01 mm/Hg), 31.3 g of 2-ethyl-3-acetyl-benzo[b]thiophene
出典と根拠
- ORDレコード
- ord-5cae08587a4f456aa6d3280aeaaa1394
- 出典データセット
- uspto-grants-1977_02
- 特許番号
- US04007204
関連ノート
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