反応式
C([C:4]1[CH:12]=[CH:11][C:10]2[NH:9][CH2:8][CH:7]3CC(N(CCC)CCC)C[C:5]=1[C:6]=23)(=O)C.C([N:25]([CH2:28]C)CC)C.ClC(OCC(Cl)(Cl)Cl)=[O:32]>C(Cl)Cl>[C:28]([N:9]1[C:10]2[C:6](=[CH:5][CH:4]=[CH:12][CH:11]=2)[CH2:7][CH2:8]1)(=[O:32])[NH2:25]参加物
5
実験手順
To a solution of (±)-6-acetyl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole (2.3 g, 7.7 mmol) and triethylamine (1.1 ml, 8 mmol) in 90 ml CH2Cl2 under N2 was added dropwise a solution of 2,2,2-trichloroethyl chloroformate. The reaction mixture was stirred at room temperature for 1 hr. The CH2Cl2 solution was extracted with water and 1N HCl. The organic solution was washed with a saturated NaHCO3 solution and with a brine solution. The CH2Cl2 solution was dried (MgSO4) and concentrated in vacuo to give 3.3 g of the 1-carbamylindoline.
後処理
- extractionThe CH2Cl2 solution was extracted with water and 1N HCl
- washThe organic solution was washed with a saturated NaHCO3 solution and with a brine solution
- dry with materialThe CH2Cl2 solution was dried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-b483a291e9eb4a43811ec149ac543b50
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05624944
関連ノート
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