반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH:9]([C:11]2[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=2)[C:14]([OH:16])=O)[CH3:10])[CH:5]=[N:4][CH:3]=1.[CH3:20][C:21]1[CH:22]=[C:23]([NH2:27])[CH:24]=[N:25][CH:26]=1.Cl.CN(C)CCCN=C=NCC.N1(C2C=CN=CC=2)CCCC1.C(N(CC)CC)C>ClCCl>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH:9]([C:11]2[CH:12]=[C:13]([CH:17]=[CH:18][CH:19]=2)[C:14]([NH:27][C:23]2[CH:24]=[N:25][CH:26]=[C:21]([CH3:20])[CH:22]=2)=[O:16])[CH3:10])[CH:5]=[N:4][CH:3]=1참가 물질
반응물 5
생성물 1
시약·촉매·용매 1
실험 절차
A mixture of 3-{1-[(6-chloropyrazin-2-yl)amino]ethyl}benzoic acid (11 mg, 0.04 mmol), 5-methylpyridin-3-amine (5 mg, 0.048 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (11 mg, 0.059 mmol), 4-pyrrolidinopyridine (1.2 mg, 0.008 mmol) and triethylamine (0.013 mL, 0.095 mmol) in dichloromethane (1 mL) was stirred at room temperature for 17 hours. After this time the mixture was diluted with dichloromethane (20 mL), washed successively with saturated aqueous sodium hydrogen carbonate (2×15 mL) and brine (15 mL), dried (Na2SO4) and concentrated under reduced pressure to give a dark yellow oil which was purified by flash chromatography (silica, ethyl acetate/methanol) to give 3-{1-[(6-chloropyrazin-2-yl)amino]ethyl}-N-(5-methylpyridin-3-yl)benzamide (9 mg, 61%) as a pale yellow oil.
후처리
- washwashed successively with saturated aqueous sodium hydrogen carbonate (2×15 mL) and brine (15 mL)
- dry with materialdried (Na2SO4)
- concentrationconcentrated under reduced pressure
- customto give a dark yellow oil which
- customwas purified by flash chromatography (silica, ethyl acetate/methanol)
출처 및 근거
- ORD 기록
- ord-54eb7710c91b4e22b485ec28d903e918
- 출처 데이터셋
- uspto-grants-2015_05
- 특허 번호
- US09029386B2
연결된 노트
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