3-Aminopicolinic acid → Methyl 3-aminopyridine-2-carboxylate
反応式
[NH2:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[CH3:11][Si](C=[N+]=[N-])(C)C>CO.C(OCC)C.C(OCC)(=O)C>[CH3:11][O:9][C:8]([C:3]1[C:2]([NH2:1])=[CH:7][CH:6]=[CH:5][N:4]=1)=[O:10]参加物
6
実験手順
400 mg (2.9 mmol) of 3-amino-pyridine-2-carboxylic acid was dissolved in 3 mL of methanol. To this solution 1.6 mL of 2 M (trimethylsilyl)diazomethane solution in diethyl ether was added dropwise at 0° C., followed by stirring of the mixture for 2 hours at room temperature The solution was diluted with ethyl acetate and washed with aqueous sodium bicarbonate solution. Flash chromatography afforded the ester product. LC-MSD, m/z for C7H8N2O2 [M+H]+=153.0; HPLC retention time: 0.2 minutes.
後処理
- washwashed with aqueous sodium bicarbonate solution
出典と根拠
- ORDレコード
- ord-69e5ce582b7c4b4fbe61df9d1fd05af6
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08546408B2
反応ノート
読み込み中…