Sodium hydride → 2,6-Diamino-4,5-dihydronicotinic acid ethyl ester
반응식
[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]참가 물질
4
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-8ac65dab0bd542bcb47fb687edd02869
- 출처 데이터셋
- uspto-grants-2012_05
- 특허 번호
- US08183264B2
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