Hydrochloric Acid → HCID 178527533, Verbindung
Reaktionsgleichung
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:41]=[CH:40][C:39]([F:42])=[CH:38][C:37]=1[C:43]([F:46])([F:45])[F:44])(=[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:41]=[CH:40][C:39]([F:42])=[CH:38][C:37]=4[C:43]([F:46])([F:44])[F:45])(=[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]=1Komponenten
3
Versuchsvorschrift
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)-4-fluoro-2-(trifluoromethyl)benzenesulfonamide (20 mg, 0.031 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 16 mg of the target compound, N-(3-(3-(9H-purin-6-yl)pyridin-2-ylamino)-2,4-difluorophenyl)-4-fluoro-2-(trifluoromethyl)benzenesulfonamide (percentage yield: 90%), was obtained.
Aufarbeitung
- 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
Quellen und Nachweise
- ORD-Eintrag
- ord-bc65b1e64530411e896eb78c7d96bb52
- Quelldatensatz
- uspto-grants-2015_12
- Patentnummer
- US09216981B2
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