Hydrochloric Acid → 2-Hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin

HRID 903636

반응식

HRID 903636 반응식
[OH:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][C:7]3[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([OH:17])=[O:16])[C:8]=3[CH2:9][CH2:10][C:4]=2[CH:3]=1.Cl.[CH2:21](O)[CH3:22]>C(OCC)(=O)C.C1C=CC=CC=1>[OH:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][C:7]3[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([O:17][CH2:21][CH3:22])=[O:16])[C:8]=3[CH2:9][CH2:10][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 233370412-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin

생성물 1

HCID 126871252-Hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin수율 85%

시약·촉매·용매 1

HCID 21583983Benzene ethyl acetate용매

실험 절차

An amount of 1.7 g of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin was dissolved in 50ml of anhydrous ethanol and the mixture was refluxed for 3 hours, while hydrogen chloride gas was bubbled into the mixture. The solvent was distilled off to obtain the residue which was dissolved in the mixed solvent of ethyl acetate-benzene. The solution was washed with saturated sodium chloride solution and freed of solvent by distillation to obtain 1.6 g (85%) of 2-hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 125°-129° C.

후처리

  1. customwas bubbled into the mixture
  2. distillationThe solvent was distilled off
  3. customto obtain the residue which
  4. washThe solution was washed with saturated sodium chloride solution
  5. distillationfreed of solvent by distillation

출처 및 근거

ORD 기록
ord-07fce35fe7bc4323945a6a1017ceb78e
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04228284

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