반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([OH:9])=O)=[C:3]([C:10]([OH:12])=O)[CH:2]=1.O.ON1[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2N=N1.[C:24]1([CH2:30][CH2:31][CH2:32][CH2:33][NH2:34])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C([N:37]([CH2:40][CH3:41])CC)C.Cl.CN(C)[CH2:45][CH2:46]CN=C=NCC>CN(C=O)C>[C:18]1([CH2:45][CH2:46][CH2:41][CH2:40][NH:37][C:10]([C:3]2[CH:2]=[N:1][CH:6]=[CH:5][C:4]=2[C:7]([NH:34][CH2:33][CH2:32][CH2:31][CH2:30][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:9])=[O:12])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1참가 물질
반응물 5
생성물 1
시약·촉매·용매 1
실험 절차
3,4-Pyridinedicarboxylic acid (1 g; 6.0 mmol) is slurried in DMF (50 mL) at ambient temperature. To this reaction mixture is added sequentially 1-hydroxybenzotriazole hydrate (2.43 g; 18.0 mmol), 4-phenylbutylamine (2.08 mL; 13.2 mmol), triethylamine (1.67 mL; 12.0 mmol), and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (2.87 g; 15.0 mmol). The reaction mixture is stirred for 18 hours at ambient temperature. The batch is poured onto ethyl acetate (300 mL), then extracted sequentially with water (100 mL), 1N HCl (100 mL), saturated aqueous sodium bicarbonate (50 mL), and brine (50 mL). The organic phase is dried over MgSO4, filtered, and concentrated in vacuo affording the desired product (2.65 g) as a semi-solid. ESMS: MH+ 430.0.
후처리
- additionThe batch is poured onto ethyl acetate (300 mL)
- extractionextracted sequentially with water (100 mL), 1N HCl (100 mL), saturated aqueous sodium bicarbonate (50 mL), and brine (50 mL)
- dry with materialThe organic phase is dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-444ef3a4d4a34159ba514961f4fdf438
- 출처 데이터셋
- uspto-grants-2009_01
- 특허 번호
- US07476680B2
연결된 노트
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