반응식
C(O)C.[CH3:4][N:5]([CH2:7][C:8]1[S:12][C:11]([CH2:13][S:14][CH2:15][CH2:16][NH:17][C:18](SC)=[CH:19][N+:20]([O-:22])=[O:21])=[CH:10][C:9]=1[CH3:25])[CH3:6].[Br:26][C:27]1[CH:28]=[C:29]([CH:33]([OH:36])[CH2:34][NH2:35])[CH:30]=[CH:31][CH:32]=1.C(O)(C)C>C(OCC)C>[Br:26][C:27]1[CH:28]=[C:29]([CH:33]([OH:36])[CH2:34][NH:35][C:18]([NH:17][CH2:16][CH2:15][S:14][CH2:13][C:11]2[S:12][C:8]([CH2:7][N:5]([CH3:4])[CH3:6])=[C:9]([CH3:25])[CH:10]=2)=[CH:19][N+:20]([O-:22])=[O:21])[CH:30]=[CH:31][CH:32]=1참가 물질
6
실험 절차
With 7.5 ml of ethanol were mixed 4.5 g of 1-{2-[[5-(dimethylamino)methyl-4-methyl-2-thienyl]methylthio]ethylamino}-1-methylthio-2-nitroethene and 3.5 g of DL-[2-(3-bromophenyl)-2-hydroxyethyl]amine, and the resulting mixture was subjected to reaction at room temperature for 30 hours. Thereto were added 5 ml of isopropanol and 30 ml of diethyl ether, and the mixture thus obtained was stirred, after which the crystals formed were collected by filtration. The crystals were recrystallized from 40 ml of isopropanol to obtain 4.3 g (yield 65%) of N-[2-(3-bromophenyl)-2-hydroxyethyl]-N'-{2-[[5-(dimethylamino)methyl-4-methyl-2-thienyl]methylthio]ethyl}-2-nitro-1,1-ethenediamine having a melting point of 104°-106° C.
후처리
- customthe resulting mixture was subjected to reaction at room temperature for 30 hours
- customthe mixture thus obtained
- customafter which the crystals formed
- filtrationwere collected by filtration
- customThe crystals were recrystallized from 40 ml of isopropanol
출처 및 근거
- ORD 기록
- ord-59cc1cc09f514814abfa4ab4111f84d8
- 출처 데이터셋
- uspto-grants-1990_05
- 특허 번호
- US04923882
연결된 노트
불러오는 중…