Lithium Hydroxide → Benzoic Acid
反応式
O(C1C=CC(NC2N=CN=C(N[C:22]3[CH:23]=[C:24]([CH:29]=[CH:30][CH:31]=3)[C:25]([O:27]C)=[O:26])C=2)=CC=1)C1C=CC=CC=1.[Li+].[OH-]>CO.C1COCC1.O>[C:25]([OH:27])(=[O:26])[C:24]1[CH:29]=[CH:30][CH:31]=[CH:22][CH:23]=1参加物
5
実験手順
To a stirred solution of methyl 3-(6-(4-phenoxyphenylamino)pyrimidin-4-ylamino)benzoate (0.3 g, 0.72 mmol) in methanol/THF (2/2, 4 mL) was added LiOH (0.122 g, 2.9 mmol) in H2O (4 mL) and the reaction mixture was stirred at rt for 2 h. It was concentrated under reduced pressure. the residue was diluted with water (2 mL) and was extracted with dichloromethane (5 mL). The aqueous layer was separated and was acidified with 1.5 N HCl (pH ˜5-6) to get a white precipitate, which was collected by filtration and dried under vacuum to give 34644-phenoxyphenylamino)pyrimidin-4-ylamino)benzoic acid (0.2 g 69%) as a white solid.
後処理
- concentrationIt was concentrated under reduced pressure
- additionthe residue was diluted with water (2 mL)
- extractionwas extracted with dichloromethane (5 mL)
- customThe aqueous layer was separated
- customto get a white precipitate, which
- filtrationwas collected by filtration
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-1ffd5243c25e4cdf88c289647e234524
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040541B2
反応ノート
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