1,2-Dichloroethane → 5-Bromo-N-methylpyridine-2-carboxamide
反応式
[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]=1参加物
8
実験手順
5-Bromo-2-pyridinecarboxylic acid (D10) (1 g) was dissolved in dry DMF (50 ml) and treated with methylamine hydrochloride (0.42 g), EDC (1.2 g), 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+).
後処理
- extractionextracted with DCM (50 ml)
- extractionThe organic extract
- washwas washed with brine (5×50 ml)
- dry with materialdried (magnesium sulfate)
- customevaporated
出典と根拠
- ORDレコード
- ord-951e4bbe6dca4b4d9a1b69c725d0796c
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08492375B2
反応ノート
読み込み中…
