Hydrochloric Acid → HCID 178429734、化合物
反応式
Cl.[F:2][C:3]1[C:8]([NH:9][C:10]2[C:15]([C:16]3[N:24]=[CH:23][N:22]=[C:21]4[C:17]=3[N:18]=[CH:19][N:20]4C3CCCCO3)=[CH:14][CH:13]=[CH:12][N:11]=2)=[C:7]([F:31])[CH:6]=[CH:5][C:4]=1[NH:32][S:33]([C:36]1[CH:40]=[C:39]([CH3:41])[O:38][C:37]=1[C:42]([F:45])([F:44])[F:43])(=[O:35])=[O:34]>>[N:24]1[C:16]([C:15]2[C:10]([NH:9][C:8]3[C:3]([F:2])=[C:4]([NH:32][S:33]([C:36]4[CH:40]=[C:39]([CH3:41])[O:38][C:37]=4[C:42]([F:45])([F:44])[F:43])(=[O:35])=[O:34])[CH:5]=[CH:6][C:7]=3[F:31])=[N:11][CH:12]=[CH:13][CH:14]=2)=[C:17]2[C:21]([NH:20][CH:19]=[N:18]2)=[N:22][CH:23]=1参加物
3
実験手順
1M aqueous hydrochloric acid solution was added into the N-(2,4-difluoro-3-(3-(9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-yl)pyridin-2-ylamino)phenyl)-5-methyl-2-(trifluoromethyl)furan-3-sulfonamide (12 mg, 0.020 mmol) prepared at Step 10 and stirred for 2 hours. After the reaction, the reactant was washed with an aqueous solution of sodium hydrogen carbonate and salt water. After extraction with ethylacetate, the organic layer was dried with sulfuric anhydride magnesium and vacuum concentrated, and then refined by means of column chromatography, so that 9 mg of the target compound, N-(3-(3-(9H-purin-6-yl)pyridin-2-ylamino)-2,4-difluorophenyl)-5-methyl-2-(trifluoromethyl)furan-3-sulfonamide (percentage yield: 85%), was obtained.
後処理
- customprepared at Step 10
- customAfter the reaction
- washthe reactant was washed with an aqueous solution of sodium hydrogen carbonate and salt water
- extractionAfter extraction with ethylacetate
- dry with materialthe organic layer was dried with sulfuric anhydride magnesium and vacuum
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6c02e65179254fe4a9e3d34c45727fa3
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09216981B2
反応ノート
読み込み中…