Sulfuric acid magnesium salt (1:1) → 1-Benzyl 4-tert-butyl 2-[(4-{[(3,4-dichlorophenyl)amino]carbonyl}piperazin-1-yl)methyl]piperazine-1,4-dicarboxylate

HRID 603228

反応式

HRID 603228 の反応式
[CH:1]([CH:3]1[CH2:8][N:7]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:6][CH2:5][N:4]1[C:16]([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17])=O.[Cl:26][C:27]1[CH:28]=[C:29]([NH:34][C:35]([N:37]2[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)=[O:36])[CH:30]=[CH:31][C:32]=1[Cl:33].CCN(C(C)C)C(C)C.[O-]S([O-])(=O)=O.[Mg+2].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>C1COCC1.C(OCC)(=O)C>[Cl:26][C:27]1[CH:28]=[C:29]([NH:34][C:35]([N:37]2[CH2:42][CH2:41][N:40]([CH2:1][CH:3]3[CH2:8][N:7]([C:9]([O:11][C:12]([CH3:13])([CH3:14])[CH3:15])=[O:10])[CH2:6][CH2:5][N:4]3[C:16]([O:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:17])[CH2:39][CH2:38]2)=[O:36])[CH:30]=[CH:31][C:32]=1[Cl:33]

参加物

9

反応物 6

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 16775732N-(3,4-Dichlorophenyl)piperazine-1-carboxamideHCID 596715274-Boc-1-Cbz-piperazine-2-carbaldehyde

生成物 1

HCID 576568421-Benzyl 4-tert-butyl 2-[(4-{[(3,4-dichlorophenyl)amino]carbonyl}piperazin-1-yl)methyl]piperazine-1,4-dicarboxylate

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To 1-benzyl 4-tert-butyl 2-formylpiperazine-1,4-dicarboxylate (227 mg) in THF (20 ml) were added N-(3,4-dichlorophenyl)piperazine-1-carboxamide (179 mg), DIPEA (319 ul) DMF (1.6 ml) and MgSO4 (30 mg) the mixture stirred at room temperature for 30 minutes, sodium triacetoxyborohydride (277 mg) added and stirring continued for 16 hours at room temperature. Saturated aqueous sodium bicarbonate and ethyl acetate were added. The organic phase was dried (MgSO4) and evaporated to give the title compound as a semi-solid gum (331 mg, 84%).

後処理

  1. stirringstirring
  2. waitcontinued for 16 hours at room temperature
  3. dry with materialThe organic phase was dried (MgSO4)
  4. customevaporated

出典と根拠

ORDレコード
ord-a7456215a8404e3184a2b6ecf57f4599
出典データセット
uspto-grants-2011_03
特許番号
US07906645B2

関連ノート

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