4-Aminopyridine → Ethyl 4-pyridinylcarbamate
反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.Cl[C:9]([O:11][CH2:12][CH3:13])=[O:10]>N1C=CC=CC=1.C(Cl)Cl>[CH2:12]([O:11][C:9]([NH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1)=[O:10])[CH3:13]参加物
5
反応条件
- 温度
- 0 °C
実験手順
4-Aminopyridine (17.34 grams) (184.3) was dissolved in dry pyridine (217 ml.) and cooled to 0° C. over 30 minutes. Ethyl chloroformate (17.2 ml.) (180.7 mmoles) was added and the solution was stirred at 0° C. for 1 hour and then at 25° C. for 40 hours. The mixture was diluted with CH2Cl2 and washed with saturated aqueous NaHCO3 and water. The CH2Cl2 was dried (MgSO4), filtered and evaporated to dryness. The residue was chromatographed on silica gel using 2% (10% saturated NH4OH in MeOH)--CH2Cl2 to give the title compound (Yield: 10 grams, 33% M+ 166).
後処理
- waitat 25° C. for 40 hours
- washwashed with saturated aqueous NaHCO3 and water
- dry with materialThe CH2Cl2 was dried (MgSO4)
- filtrationfiltered
- customevaporated to dryness
- customThe residue was chromatographed on silica gel using 2% (10% saturated NH4OH in MeOH)
出典と根拠
- ORDレコード
- ord-a53ad38342bc44adab5dc0766182ee1d
- 出典データセット
- uspto-grants-1998_02
- 特許番号
- US05714609
反応ノート
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