Iodoethane → Ethyl 2,3-dichloropyridine-4-carboxylate
反応式
[Cl:1][C:2]1[C:3]([Cl:11])=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([OH:7])=[O:6].[H-].[Na+].I[CH2:15][CH3:16]>CN(C=O)C>[CH2:15]([O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][N:10]=[C:2]([Cl:1])[C:3]=1[Cl:11])[CH3:16]参加物
5
実験手順
To a solution of 2,3-dichloroisonicotinic acid (5.62 mmol) in 15 mL DMF were added NaH (7.31 mmol) followed by iodoethane (6.75 mmol) at 0° C. The cooling bath was removed and the mixture was stirred at RT overnight. The reaction was quenched with sat. aq. NaHCO3 solution and extracted with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo. Purification by CC (KP-SIL™ from Biotage) using Hept/EtOAc (6/4) gives the desired product as yellow oil;
後処理
- customThe cooling bath was removed
- customThe reaction was quenched with sat. aq. NaHCO3 solution
- extractionextracted with EtOAc
- dry with materialThe combined organic layers were dried over MgSO4
- concentrationconcentrated in vacuo
- customPurification by CC (KP-SIL™ from Biotage)
出典と根拠
- ORDレコード
- ord-ccf9cfeb327a4e019818146ffd1f8e6d
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09221832B2
反応ノート
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