Hydrochloric Acid → HCID 178513245、化合物
反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([Br:9])=[CH:5][CH:4]=1)#[N:2].Cl.[NH2:11][OH:12].C([O-])([O-])=O.[Na+].[Na+]>CCO.O>[Br:9][C:6]1[CH:7]=[CH:8][C:3]([C:1](=[NH:2])[NH:11][OH:12])=[CH:4][CH:5]=1参加物
7
実験手順
A mixture of 4-cyano-bromobenzene (0.5 g, 2.75 mmol), HCl×NH2OH (0.476 g, 6.9 mmol) and Na2CO3 (0.731 g, 6.9 mmol) in a mixture of EtOH and H2O (25 ml: 5 ml) was stirred for 7 h at reflux. The solvent was evaporated to dryness and the residue was taken in EtOAc (100 ml) and washed with H2O. The organic layer was separated, dried over MgSO4 and filtered. The filtrate was evaporated to dryness to give the product as colourless solid (0.51 g, 87%). 1H-NMR (DMSO-d6) 5.81 (broad s, 2H); 7.53 (d, 2H, J=6.66 Hz); 7.58 (d, 2H, J=6.54 Hz); 9.69 (s, 1H).
後処理
- temperatureat reflux
- customThe solvent was evaporated to dryness
- washwashed with H2O
- customThe organic layer was separated
- dry with materialdried over MgSO4
- filtrationfiltered
- customThe filtrate was evaporated to dryness
出典と根拠
- ORDレコード
- ord-369e3b23f28f4b889b8fc860bd8c712b
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181182B2
反応ノート
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