반응식
[NH2:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][NH2:10].ClCCl.[Cl:14][C:15]1[CH:16]=[C:17]2[C:22](=[C:23]([Cl:25])[CH:24]=1)[CH2:21][N:20]([CH3:26])[CH2:19][CH:18]2[C:27]1[CH:28]=[C:29]([S:33](Cl)(=[O:35])=[O:34])[CH:30]=[CH:31][CH:32]=1>CN(C=O)C.C(OCC)(=O)C>[NH2:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][NH:10][S:33]([C:29]1[CH:30]=[CH:31][CH:32]=[C:27]([CH:18]2[C:17]3[C:22](=[C:23]([Cl:25])[CH:24]=[C:15]([Cl:14])[CH:16]=3)[CH2:21][N:20]([CH3:26])[CH2:19]2)[CH:28]=1)(=[O:35])=[O:34]참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
실험 절차
To a 50-mL 3-necked round-bottom flask was added 2-(2-(2-aminoethoxy)ethoxy)ethanamine (3.2 g, 21.59 mmol, 21.09 equiv) and dichloromethane (DCM; 20 mL). This was followed by the addition of a solution of 3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzene-1-sulfonyl chloride (Intermediate 1.6) (400 mg, 1.02 mmol, 1.00 equiv) in DMF (5 mL) dropwise with stirring. The resulting solution was stirred for 5 h at which time it was diluted with 100 mL of ethyl acetate. The resulting mixture was washed successively with 2×10 mL of water and 1×10 mL of Brine. The organic layer was dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 300 mg (58%) of N-(2-(2-(2-aminoethoxy)ethoxy)ethyl)-3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonamide as a yellow oil.
후처리
- stirringThe resulting solution was stirred for 5 h at which time it
- washThe resulting mixture was washed successively with 2×10 mL of water and 1×10 mL of Brine
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated under vacuum
- customThis resulted in 300 mg (58%) of N-(2-(2-(2-aminoethoxy)ethoxy)ethyl)-3-(6,8-dichloro-2-methyl-1,2,3,4-tetrahydroisoquinolin-4-yl)benzenesulfonamide as a yellow oil
출처 및 근거
- ORD 기록
- ord-13d4bef2d9c9446ea4d07c7383f6cb13
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08969377B2
연결된 노트
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