Hydrochloric Acid → (S)-1-(4-Chloro-3,5-dimethyl-phenyl)-2,2,2-trifluoro-ethylamine
反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([C@H:9]([NH:14][S@@](C(C)(C)C)=O)[C:10]([F:13])([F:12])[F:11])=[CH:4][C:3]=1[CH3:21].Cl>CO>[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([C@H:9]([NH2:14])[C:10]([F:12])([F:13])[F:11])=[CH:4][C:3]=1[CH3:21]参加物
4
実験手順
A solution of intermediate INT 42 (860 mg, 2.52 mmol) in MeOH (40 mL) was treated with HCl (4 M in dioxane, 1.26 mL, 5.04 mmol) and stirred over the weekend. After evaporation of the solvents, a solid was obtained which was triturated with Et2O. The solid was then dissolved in water and the pH was adjusted to ˜9 using 10% sodium carbonate solution. It was extracted twice with EtOAc. The combined extracts were dried over sodium sulfate, filtered and concentrated.
後処理
- customAfter evaporation of the solvents
- customa solid was obtained which
- customwas triturated with Et2O
- dissolutionThe solid was then dissolved in water
- extractionIt was extracted twice with EtOAc
- dry with materialThe combined extracts were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-b42165ca4eed4775a06c06d6dc78420c
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08791100B2
反応ノート
読み込み中…