反応式
F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.[F:25][C:26]1[CH:31]=[C:30]([CH2:32][S:33][C:34]2[C:39]([C:40]([OH:42])=O)=[CH:38][CH:37]=[CH:36][N:35]=2)[CH:29]=[CH:28][N:27]=1.[NH2:43][C:44]1[CH:49]=[C:48]([CH3:50])[CH:47]=[C:46]([CH3:51])[CH:45]=1.C(N(CC)C(C)C)(C)C>CN(C)C=O.C(OCC)(=O)C>[CH3:51][C:46]1[CH:45]=[C:44]([NH:43][C:40]([C:39]2[C:34]([S:33][CH2:32][C:30]3[CH:29]=[CH:28][N:27]=[C:26]([F:25])[CH:31]=3)=[N:35][CH:36]=[CH:37][CH:38]=2)=[O:42])[CH:49]=[C:48]([CH3:50])[CH:47]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
O-(7-Azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (3.0 g, 7.9 mmol) was added to a solution of 2-(2-fluoropyridin-4-ylmethylthio)pyridine-3-carboxylic acid (Reference compound No. 2-1, 1.5 g, 5.7 mmol), 3,5-xylidine (0.90 g, 7.4 mmol) and N,N-diisopropylethylamine (2.0 mL, 11 mmol) in N,N-dimethylformamide (20 mL) at room temperature, and the mixture was stirred for 12 hours. Ethyl acetate (30 mL) was added to the reaction mixture, the whole was washed with brine (50 mL), and then the organic layer was dried over anhydrous magnesium sulfate. The organic layer was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography to give 0.91 g of the title reference compound as a colorless solid. (Yield 44%)
後処理
- washthe whole was washed with brine (50 mL)
- dry with materialthe organic layer was dried over anhydrous magnesium sulfate
- customThe organic layer was evaporated under reduced pressure
- customthe resulting residue was purified by silica gel column chromatography
- customto give 0.91 g of the title reference compound as a colorless solid
出典と根拠
- ORDレコード
- ord-ea30108da48641dab223eac646c5af13
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07544703B2
関連ノート
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