Sodium hydride → 2,6-Diamino-4,5-dihydronicotinic acid ethyl ester
反応式
[H-].[Na+].[CH2:3]([O:5][C:6](=[O:15])[C:7](=[C:12]([NH2:14])[NH2:13])[CH2:8][CH2:9][C:10]#[N:11])[CH3:4]>C1COCC1>[CH2:3]([O:5][C:6]([C:7]1[CH2:8][CH2:9][C:10]([NH2:11])=[N:14][C:12]=1[NH2:13])=[O:15])[CH3:4]参加物
4
実験手順
To a suspension of THF (7 mL) and NaH (210 mg/60% in oil) was added dropwise a solution of THF (7 mL) and 4-cyano-2-diaminomethylene-butyric acid ethyl ester (0.55 g) described in Manufacturing Example 10-2-1, which was refluxed for 19 hours and 20 minutes. The reaction solution was poured into ice water and then extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, after which the solvent was evaporated under a reduced pressure to obtain the crude titled compound (0.19 g).
後処理
- temperaturewas refluxed for 19 hours and 20 minutes
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- customafter which the solvent was evaporated under a reduced pressure
出典と根拠
- ORDレコード
- ord-8ac65dab0bd542bcb47fb687edd02869
- 出典データセット
- uspto-grants-2012_05
- 特許番号
- US08183264B2
反応ノート
読み込み中…