Methyl iodide → Methyl 2-chloro-6-methylpyridine-3-carboxylate
反応式
[Cl:1][C:2]1[N:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].CI.[C:14]([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:14][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([CH3:11])=[N:10][C:2]=1[Cl:1]参加物
5
実験手順
2-Chloro-6-methyl-nicotinic acid (3.58 g, 20.86 mmol) was dissolved in DMF (34 mL). MeI (5.8 mL, 93.88 mmol) and K2CO3(7.78 g, 56.33 mmol) were added thereto, and the mixture was stirred at room temperature for 2 hours. The reactant was distilled under reduced pressure to remove the solvent and extracted with EtOAc. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure. The obtained residue was purified by column chromatography (eluent EtOAc/Hex=1/2) to obtain the title compound (3.68 g, 94%).
後処理
- distillationThe reactant was distilled under reduced pressure
- customto remove the solvent
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried with MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe obtained residue was purified by column chromatography (eluent EtOAc/Hex=1/2)
出典と根拠
- ORDレコード
- ord-fbfad6ac0e674b76aae3f5c4101743e1
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09447044B2
反応ノート
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