Water → HCID 86647413、化合物
反応式
Cl[CH2:2][C:3]1[C:4]([CH3:13])=[N:5][C:6]([CH3:12])=[C:7]([C:9]([CH3:11])=[CH2:10])[CH:8]=1.[N-:14]=[N+:15]=[N-:16].[Na+].O.CCOC(C)=O>CN(C=O)C>[N:14]([CH2:2][C:3]1[C:4]([CH3:13])=[N:5][C:6]([CH3:12])=[C:7]([C:9]([CH3:11])=[CH2:10])[CH:8]=1)=[N+:15]=[N-:16]参加物
6
反応条件
- 温度
- 70 °C
実験手順
A mixture of 96.5 mg of the 3-(chloromethyl)-2,6-dimethyl-5-(prop-1-en-2-yl)pyridine and 86.8 mg (1.34 mmol) of NaN3 in 3 mL of DMF was heated at 70° C. for 4 h. Water and EtOAc were added, and the layers were separated. The organic layer was washed with H2O (2×) and then with brine. It was dried over Na2SO4, filtered, and concentrated to give the crude azide (3-(azidomethyl)-2,6-dimethyl-5-(prop-1-en-2-yl)pyridine) which was used without further purification.
後処理
- customthe layers were separated
- washThe organic layer was washed with H2O (2×)
- dry with materialIt was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-435f5a11b9c54a84ae187c5b90f43d93
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08299267B2
反応ノート
読み込み中…