Hydrogen Bromide → 7-Hydroxy-3-piperidino-2,2-dimethylbenzofuran

HRID 3774

반응식

HRID 3774 반응식
C[O:2][C:3]1[C:11]2[O:10][C:9]([CH3:13])([CH3:12])[CH:8]([N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[C:7]=2[CH:6]=[CH:5][CH:4]=1.Br>C(O)(=O)C>[OH:2][C:3]1[C:11]2[O:10][C:9]([CH3:12])([CH3:13])[CH:8]([N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[C:7]=2[CH:6]=[CH:5][CH:4]=1

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 141266497-Methoxy-3-piperidino-2,2-dimethylbenzofuran

생성물 1

HCID 141266507-Hydroxy-3-piperidino-2,2-dimethylbenzofuran

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

7-Methoxy-3-piperidino-2,2-dimethylbenzofuran (65.1 g) is added to a stirred mixture of glacial acetic acid (340 ml) and 48% HBr (340 ml) and the solution refluxed for 3 hours. The reaction mixture is poured into crushed ice/H2O and brought to a pH=8-10. The alkaline reaction mixture is extracted with methylene chloride and the organic phase washed with water, dried, filtered and evaporated in vacuo. The residue is chromatographed on silica gel eluting with ethyl acetate/hexane (1:3) affording the desired product as a liquid.

후처리

  1. temperaturethe solution refluxed for 3 hours
  2. additionThe reaction mixture is poured
  3. customThe alkaline reaction mixture
  4. extractionis extracted with methylene chloride
  5. washthe organic phase washed with water
  6. customdried
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customThe residue is chromatographed on silica gel eluting with ethyl acetate/hexane (1:3)

출처 및 근거

ORD 기록
ord-62c89f061fa24da181f2e8c2e39d52b5
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722925

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