methyl 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-tert-butoxycarbonylpiperazine-2-carboxylate → methyl 1-(2,3-dimethoxy-6,7-dihydro-5H-benzo-cyclohepten-8-ylcarbonyl}piperazine-2-carboxylate hydrochloride

HRID 358771노트

반응식

HRID 358771 반응식
[CH3:1][O:2][C:3]1[C:4]([O:33][CH3:34])=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][C:9]([C:13]([N:15]3[CH2:20][CH2:19][N:18](C(OC(C)(C)C)=O)[CH2:17][CH:16]3[C:28]([O:30][CH3:31])=[O:29])=[O:14])=[CH:8][C:7]=2[CH:32]=1.[ClH:35].C(OCC)(=O)C>>[ClH:35].[CH3:1][O:2][C:3]1[C:4]([O:33][CH3:34])=[CH:5][C:6]2[CH2:12][CH2:11][CH2:10][C:9]([C:13]([N:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH:16]3[C:28]([O:30][CH3:31])=[O:29])=[O:14])=[CH:8][C:7]=2[CH:32]=1

참가 물질

3

반응물 2

HCID 20066655methyl 1-(2,3-dimethoxy-6,7-dihydro-5H-benzocyclohepten-8-ylcarbonyl)-4-tert-butoxycarbonylpiperazine-2-carboxylateHCID 21866389Hydrogen chloride-ethyl acetate

생성물 1

HCID 20066634methyl 1-(2,3-dimethoxy-6,7-dihydro-5H-benzo-cyclohepten-8-ylcarbonyl}piperazine-2-carboxylate hydrochloride

실험 절차

To a solution of 4.5N HCl-ethyl acetate solution (10 ml) is added methyl 1-(2,3-dimethoxy-6,7-dihydro- 5H-benzocyclohepten-8-ylcarbonyl)-4-tert-butoxycarbonylpiperazine-2-carboxylate (1.7 g). The reaction mixture is left standing at room temperature for 5 hours. Then the solvent is distilled off under reduced pressure. To the residue is added ethyl ether. Resulting precipitates are collected and dried to afford methyl 1-(2,3-dimethoxy-6,7-dihydro-5H-benzo-cyclohepten-8-ylcarbonyl}piperazine-2-carboxylate hydrochloride as colorless powder (1.2 g).

후처리

  1. waitThe reaction mixture is left
  2. distillationThen the solvent is distilled off under reduced pressure
  3. additionTo the residue is added ethyl ether
  4. customResulting
  5. customprecipitates
  6. customare collected
  7. customdried

출처 및 근거

ORD 기록
ord-45e20a93bf1d41e38d5898159bc36a60
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997836

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