Methylamine → HCID 67244656、化合物
反応式
[NH2:1][C:2]1[C:3]([C:9]([OH:11])=O)=[N:4][CH:5]=[C:6]([Br:8])[CH:7]=1.[CH3:12][NH2:13]>CN(C=O)C>[NH2:1][C:2]1[C:3]([C:9]([NH:13][CH3:12])=[O:11])=[N:4][CH:5]=[C:6]([Br:8])[CH:7]=1参加物
4
実験手順
3-Amino-5-bromopyridine-2-carboxylic acid (500 mg, 2.30 mmol) and N′,N-carbonyldiimidazole (410 mg, 2.53 mmol) were stirred in DMF (5 mL) at 40° C. for 2 hours. After cooled to room temperature, methylamine (2.0 M in THF, 2.3 mL) was added thereto and further stirred at room temperature for 1 hour. The solvent was evaporated off under reduced pressure, and the residue was purified through silica gel column chromatography (chloroform/methanol=9/1 to 4/1) to obtain the intended compound (4.99 g, 94%) as a milky white solid.
後処理
- customThe solvent was evaporated off under reduced pressure
- customthe residue was purified through silica gel column chromatography (chloroform/methanol=9/1 to 4/1)
出典と根拠
- ORDレコード
- ord-efbf7b880887422fa8fe793be22c4a8e
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07960394B2
反応ノート
読み込み中…