Ammonium Hydroxide → 3-Amino-5-chloropyridine-2-carboxamide
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N+:10]([O-])=O)[C:5]([C:8]#[N:9])=[N:6][CH:7]=1.[OH-].[NH4+].S(S([O-])=O)([O-])=[O:16].[Na+].[Na+]>O>[NH2:10][C:4]1[C:5]([C:8]([NH2:9])=[O:16])=[N:6][CH:7]=[C:2]([Cl:1])[CH:3]=1参加物
5
実験手順
To a suspension of 5-chloro-2-cyano-3-nitropyridine (1.274 mL, 10.9 mmol) in water (22 mL) was added 28% aqueous ammonium hydroxide (3.94 mL, 28.3 mmol), and the reaction was stirred at RT for 20 minutes. Sodium hydrosulfite (2.68 mL, 32.7 mmol) was added, and the reaction mixture was stirred at RT for 70 minutes. The yellow precipitate was collected by vacuum filtration to provide the title compound (1.097 g, 6.39 mmol) as yellow solid. 1H-NMR (400 MHz, DMSO-d6): δ 7.88 (br. s, 1H), δ7.73 (s, 1H), δ7.39 (br. s, 1H), δ7.23 (s, 1H), δ7.06 (br. s, 2H). LC/MS (ESI+) m/z=172 (M+H)+.
後処理
- stirringthe reaction mixture was stirred at RT for 70 minutes
- filtrationThe yellow precipitate was collected by vacuum filtration
出典と根拠
- ORDレコード
- ord-2b17b58397a14c079b7210167df35318
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09085576B2
反応ノート
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