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 358771ノート

反応式

HRID 358771 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-45e20a93bf1d41e38d5898159bc36a60
出典データセット
uspto-grants-1991_03
特許番号
US04997836

反応ノート

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