反応式
[C:1]([C:9]1[N:14]=[C:13]([CH2:15][OH:16])[CH:12]=[CH:11][CH:10]=1)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].NN>C(O)COCCOCCO>[CH2:1]([C:9]1[N:14]=[C:13]([CH2:15][OH:16])[CH:12]=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
5
実験手順
A mixture of (6-benzoyl-2-pyridyl)methanol (1.5 g, 7 mmol), potassium hydroxide (1.3 g, 23 mmol) and hydrazine 85% (1 ml, 25 mmol) in triethylene glycol (10 ml) is refluxed for 11/2 hours, and then the water and excess hydrazine are removed by a takeoff condenser until the temperature rises to 195°-200°. After 4 hours at 195°-200°, the solution is cooled, poured into ice and water (50 ml) and extracted with ether (3×20 ml). The combined ether layers are washed with water (3×20 ml), brine (10 ml) and dried over calcium sulfate. Removal of solvents gives (6-benzyl-2-pyridyl)methanol.
後処理
- temperatureis refluxed for 11/2 hours
- customthe water and excess hydrazine are removed by a takeoff condenser until the temperature
- customrises to 195°-200°
- temperaturethe solution is cooled
- additionpoured into ice and water (50 ml)
- extractionextracted with ether (3×20 ml)
- washThe combined ether layers are washed with water (3×20 ml), brine (10 ml)
- dry with materialdried over calcium sulfate
- customRemoval of solvents
出典と根拠
- ORDレコード
- ord-e5fa55e5d11d47038609d1a40afb8733
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04224330
関連ノート
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