反応式
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N-:17]=[N+:18]=[N-:19].[Na+].[Cl-].[NH4+].[OH-].[Na+]>CN(C)C=O>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([C:13]2[N:17]=[N:18][NH:19][N:14]=2)=[CH:15][CH:16]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
6
反応条件
- 温度
- 110 °C
実験手順
To a solution of 4-benzyloxybenzonitrile (2.0 g) in dimethylformamide (15 mL) were added sodium azide (932 mg) and ammonium chloride (767 mg). The mixture was stirred at 110° C. overnight under heating and then allowed to stand for cooling to room temperature. 1N aqueous sodium hydroxide was added thereto to adjust the pH to about 10, followed by washing with diethyl ether. To the aqueous layer was added 1N hydrochloric acid, and the resulting precipitated solid was filtered to give the title compound (2.29 g).
後処理
- temperatureunder heating
- temperaturefor cooling to room temperature
- washby washing with diethyl ether
- additionTo the aqueous layer was added 1N hydrochloric acid
- customthe resulting precipitated solid
- filtrationwas filtered
出典と根拠
- ORDレコード
- ord-aa7d65929a8b4b7f87d2782eda47a500
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08101774B2
関連ノート
読み込み中…