Hydrochloric Acid → 2-Chloro-4-methylpyridine-3-carboxylic acid
反応式
[Cl:1][C:2]1[N:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:3]=1[C:4]([O:6]CC)=[O:5].[OH-].[Na+].Cl>C(O)C>[Cl:1][C:2]1[N:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:3]=1[C:4]([OH:6])=[O:5]参加物
5
実験手順
A mixture of 21.8 g (0.109 mole) of ethyl 2-chloro-4-methyl-nicotinate (6) and 55 mL of a 2N-sodium hydroxide solution in 20 mL of ethanol, was refluxed for 8 hours. The solution was acidified with 2N hydrochloric acid and extracted with ether. The organic phase was dried over magnesium sulfate, filtered and concentrated to give 14.8 g (79%) of 2-chloro-4-methylnicotinic acid (7)- as a white solid, mp: 152-154° C., MS (MH)+ 172, NMR (DMSO) ppm: 2.34 (s,3H); 7.39 (d,1H); 8.33 (d,1H); 14.0 (bs COOH).
後処理
- temperaturewas refluxed for 8 hours
- extractionextracted with ether
- dry with materialThe organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-31c173b91c5a4ba49c2d9ab3069c523f
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06136982
反応ノート
読み込み中…