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 358771Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 358771
[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

Komponenten

3

Edukt 2

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

Produkt 1

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

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-45e20a93bf1d41e38d5898159bc36a60
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US04997836

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