Methanol → Methyl 6-chloropicolinate
反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=1.[CH3:11]N(C=O)C.C(Cl)(=O)C(Cl)=O.CO>C(Cl)Cl>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[CH:4][CH:3]=1参加物
6
実験手順
6-Chloropyridine-2-carboxylic acid (15.0 g, 0.11 mol) was dissolved in DCM (300 mL) and DMF (1.5 mL) and oxalyl chloride (27.4 g, 0.22 mol) was added dropwise over 10 min. The reaction mixture was stirred for 1 h, MeOH (50 mL) was added dropwise over 5 min and the reaction mixture was stirred for 1.5 h. The solvents were removed in vacuo and the residue azeotroped with DCM (2×150 mL) to give the crude title compound (16.5 g, 100%) as a green solid. LCMS (ES+): 154.5 [MH]+.
後処理
- stirringthe reaction mixture was stirred for 1.5 h
- customThe solvents were removed in vacuo
- customthe residue azeotroped with DCM (2×150 mL)
出典と根拠
- ORDレコード
- ord-4d44347bd2f84c08b3b5e9e8af8137c5
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09353086B2
反応ノート
読み込み中…