反応式
[N:1]([CH3:4])=[C:2]=[S:3].[NH2:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[N:16]([CH2:24][C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=3)[C:17]3[C:22]([N:23]=2)=[CH:21][N:20]=[CH:19][N:18]=3)[CH2:10][CH2:9]1>O1CCCC1>[F:31][C:28]1[CH:27]=[CH:26][C:25]([CH2:24][N:16]2[C:15]([NH:14][CH:11]3[CH2:10][CH2:9][N:8]([CH2:7][CH2:6][NH:5][C:2]([NH:1][CH3:4])=[S:3])[CH2:13][CH2:12]3)=[N:23][C:22]3[C:17]2=[N:18][CH:19]=[N:20][CH:21]=3)=[CH:30][CH:29]=1参加物
4
実験手順
A mixture of 0.7 parts of isothiocyanatomethane, 3.7 parts of N-[1-(2-aminoethyl)-4-piperidinyl]-9-[(4-fluorophenyl)methyl]-9H-purin-8-amine and 90 parts of tetrahydrofuran was stirred for 4 hours at room temperature. After evaporation, the residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (95:5 by volume) as eluent. The first fraction was collected and the eluent was evaporated. The residue was crystallized from acetonitrile. The product was filtered off and dried, yielding 1.3 parts (29%) of N-[2-[4-[[9-[(4-fluorophenyl)methyl]-9H-purin-8-yl]amino]-1-piperidinyl]ethyl]-N'-methylthiourea; mp. 205.5° C. (compound 179).
後処理
- customAfter evaporation
- customthe residue was purified by column chromatography over silica gel using
- additiona mixture of trichloromethane and methanol
- customThe first fraction was collected
- customthe eluent was evaporated
- customThe residue was crystallized from acetonitrile
- filtrationThe product was filtered off
- customdried
出典と根拠
- ORDレコード
- ord-9295cb5107844e6fbcfdc0eb1c8f4178
- 出典データセット
- uspto-grants-1993_11
- 特許番号
- US05258380
関連ノート
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