Methanol → Methyl 6-chloropicolinate
반응식
[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]=1참가 물질
6
실험 절차
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]+.
후처리
- stirringthe reaction mixture was stirred for 1.5 h
- customThe solvents were removed in vacuo
- customthe residue azeotroped with DCM (2×150 mL)
출처 및 근거
- ORD 기록
- ord-4d44347bd2f84c08b3b5e9e8af8137c5
- 출처 데이터셋
- uspto-grants-2016_05
- 특허 번호
- US09353086B2
반응 노트
불러오는 중…