Ethanol → Ethyl 2-chloroisonicotinate
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([OH:7])=[O:6].[CH2:11](O)[CH3:12].OS(O)(=O)=O>C(OCC)(=O)C>[CH2:11]([O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][N:10]=[C:2]([Cl:1])[CH:3]=1)[CH3:12]参加物
5
実験手順
The mixture of 2-chloro-isonicotinic acid (16.8 g, 0.107 mol), 100 mL absolute ethanol and concentrate H2SO4 (3.28 mL, 0.118 mol) was refluxed under nitrogen for 15 h. After all starting material converted, the mixture was cool down to rt, and vacuumed down all ethanol. The resulted mixture was diluted with 250 mL ethyl acetate, washed with sat. NaHCO3, dried over anhydrous Na2SO4. Purified by a short column, the 2-chloro-isonicotinic acid ethyl ester was obtained in as a pale yellow liquid. MS (ES+): 186 (M+H)+.
後処理
- temperaturewas refluxed under nitrogen for 15 h
- washwashed with sat. NaHCO3
- dry with materialdried over anhydrous Na2SO4
- customPurified by a short column
出典と根拠
- ORDレコード
- ord-9810df5ffbfb4cdfb59ada94e8985ce3
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07582631B2
反応ノート
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