3-Chloro-N,N-dimethyl-1-propanamine → 9-(3-Dimethylaminopropyl)-1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole
반응식
[CH3:1][C:2]1[C:6]2=[C:7]3[C:11](=[CH:12][CH:13]=[C:5]2[S:4][CH:3]=1)[NH:10][C:9]1[CH2:14][CH2:15][NH:16][CH2:17][C:8]3=1.[CH3:18][N:19]([CH3:24])[CH2:20][CH2:21][CH2:22]Cl>CN(C)C=O>[CH3:18][N:19]([CH3:24])[CH2:20][CH2:21][CH2:22][N:16]1[CH2:15][CH2:14][C:9]2[NH:10][C:11]3[C:7]([C:8]=2[CH2:17]1)=[C:6]1[C:2]([CH3:1])=[CH:3][S:4][C:5]1=[CH:13][CH:12]=3참가 물질
4
실험 절차
10 g of 1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole, dissolved in 200 ml of dimethylformamide at 90° C., are heated to 90° with a solution of 12 ml of 3-dimethylaminopropyl chloride in 50 ml of dimethylformamide for 3 hours. The reaction mixture is filtered, the filtrate is evaporated and the residue is taken up in chloroform. After washing with water and drying, the organic phase is concentrated, the residue is chromatographed on SiO2 with chloroform/methanol/NH4OH (7:3:0:1) and the product is recrystallised from isopropanol. Melting point: 184° C.
후처리
- filtrationThe reaction mixture is filtered
- customthe filtrate is evaporated
- washAfter washing with water
- customdrying
- concentrationthe organic phase is concentrated
- customthe residue is chromatographed on SiO2 with chloroform/methanol/NH4OH (7:3:0:1)
- customthe product is recrystallised from isopropanol
출처 및 근거
- ORD 기록
- ord-623cd7677ddf4e8fb8633c361bf4b97d
- 출처 데이터셋
- uspto-grants-1983_10
- 특허 번호
- US04410536
반응 노트
불러오는 중…