Hydrochloric Acid → 2-Ethyl-3-acetyl-benzo[b]thiophene

HRID 436005

반응식

HRID 436005 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 5956642-Ethylbenzo[b]thiophene

생성물 1

HCID 214550882-Ethyl-3-acetyl-benzo[b]thiophene수율 765%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

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%.

후처리

  1. customInto a one-litre flask fitted with a mechanical stirrer and a dropping-funnel
  2. temperatureAfter the solution was cooled to between 5 and 10° C by means of an ice-bath
  3. customto return to room temperature
  4. customThe complex so formed
  5. customThe organic and aqueous phases were separated by decantation
  6. extractionthe aqueous phase was extracted with ether
  7. additionThe ethereal fraction was then added to the organic phase
  8. washthe mixture was washed with water
  9. customevaporated to dryness
  10. customto give
  11. distillationafter distillation between 124°-134° C (0.01 mm/Hg), 31.3 g of 2-ethyl-3-acetyl-benzo[b]thiophene

출처 및 근거

ORD 기록
ord-5cae08587a4f456aa6d3280aeaaa1394
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04007204

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