1,2-Dichloroethane → 5-Bromo-N-methylpyridine-2-carboxamide
반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([OH:10])=O)=[N:6][CH:7]=1.Cl.CN.C(Cl)CCl.C1C=CC2N(O)N=[N:24][C:22]=2C=1>CN(C=O)C.O.CCN(CC)CC>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([NH:24][CH3:22])=[O:10])=[N:6][CH:7]=1참가 물질
8
실험 절차
5-Bromo-2-pyridinecarboxylic acid (D10) (1 g) was dissolved in dry DMF (50 ml) and treated with methylamine hydrochloride (0.42 g), EDC (1.29), HOBT (0.56 g) and Et3N (2.4 ml). The reaction was stirred at rt overnight then poured into water (200 ml) and extracted with DCM (50 ml). The organic extract was washed with brine (5×50 ml), dried (magnesium sulfate) and evaporated to give the title compound (D11) as a yellow crystalline solid (0.45 g). LCMS electrospray (+ve) 349 (MH+).
후처리
- extractionextracted with DCM (50 ml)
- extractionThe organic extract
- washwas washed with brine (5×50 ml)
- dry with materialdried (magnesium sulfate)
- customevaporated
출처 및 근거
- ORD 기록
- ord-176d30156a454c06bb2be00faa5993c1
- 출처 데이터셋
- uspto-grants-2010_12
- 특허 번호
- US07846922B2
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