反応式
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:21][N:22]1[C:34]2[CH2:33][CH2:32][CH:31]([CH2:35][C:36]3[N:37]=[CH:38][NH:39][C:40]=3[CH3:41])[C:30](=[O:42])[C:29]=2[C:28]2[C:23]1=[CH:24][CH:25]=[CH:26][CH:27]=2.C(N(CC)CC)C.O>CN(C=O)C>[CH3:21][N:22]1[C:34]2[CH2:33][CH2:32][CH:31]([CH2:35][C:36]3[N:37]=[CH:38][N:39]([C:7]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)([C:9]4[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=4)[C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)[C:40]=3[CH3:41])[C:30](=[O:42])[C:29]=2[C:28]2[C:23]1=[CH:24][CH:25]=[CH:26][CH:27]=2参加物
実験手順
A solution of triphenylchloromethane (286 mg) in dry DMF (10 ml) was added dropwise to a stirred solution of 1,2,3,9-tetrahydro-9-methyl-3-[(5-methyl-1H-imidazol-4-yl)methyl]-4H-carbazol-4-one (292 mg) and triethylamine (101 mg) in dry DMF (20 ml) and the resulting solution was stirred at room temperature under nitrogen for 3.5 h. The reaction mixture was then poured into water (100 ml) and the resultant suspension was extracted with dichloromethane (3×50 ml). The combined, dried organic extracts were adsorbed onto FCC silica which was then applied to a column and FCC eluting with System A (150:8:1) gave a solid which was further purified by crystallisation from dichloromethane:hexane (2:1) to give the title compound (304 mg), m.p. 193°-195°.
後処理
- extractionthe resultant suspension was extracted with dichloromethane (3×50 ml)
- washeluting with System A (150:8:1)
- customgave a solid which
- customwas further purified by crystallisation from dichloromethane:hexane (2:1)
出典と根拠
- ORDレコード
- ord-4e3771d0851b4b57a2238a9b93786062
- 出典データセット
- uspto-grants-1989_04
- 特許番号
- US04822881
関連ノート
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