Ammonium Hydroxide → 5-Iodo-2-(trifluoromethyl)pyridin-4-amine
反応式
[OH-].[NH4+:2].Cl[C:4]1[C:9]([I:10])=[CH:8][N:7]=[C:6]([C:11]([F:14])([F:13])[F:12])[CH:5]=1>CS(C)=O.[Cl-].[Na+].O>[I:10][C:9]1[C:4]([NH2:2])=[CH:5][C:6]([C:11]([F:14])([F:13])[F:12])=[N:7][CH:8]=1参加物
5
反応条件
- 温度
- 110 °C
実験手順
Concentrated aqueous ammonium hydroxide (10 mL) was added to a solution of 4-chloro-5-iodo-2-(trifluoromethyl)pyridine (4.11 g, 13.3 mmol) in DMSO in a glass pressure tube. The tube was sealed and placed in an oil bath pre-heated to 110° C. for 48 h. The resulting solution was diluted with brine, extracted with ethyl acetate, dried (Na2SO4), filtered and concentrated under vacuum to give 5-iodo-2-(trifluoromethyl)pyridin-4-amine. Retention time (min)=1.584, method [1], MS (ESI) 289.0 (M+H).
後処理
- customThe tube was sealed
- customplaced in an oil bath
- extractionextracted with ethyl acetate
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-7b8cb35540dc40b9b333e3db851d8f64
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08450363B2
反応ノート
読み込み中…