Chloroacetyl chloride → 2-chloro-N-(pyridin-2-ylmethyl)acetamide
反応式
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:15][CH2:16][C:17](Cl)=[O:18]>CC(C)=O>[Cl:15][CH2:16][C:17]([NH:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)=[O:18]参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a solution of 0.5 g (4.6 mmol) 2-(aminomethyl)pyridine in 10 ml acetone at 0° C. were added 1.27 g (9.2 mmol) potassium carbonate and 0.57 g (5.1 mmol) 2-chloro acetylchloride. The reaction was stirred at 0° C. until no starting material remained and then poured onto ice water. The mixture was extracted twice with ethyl acetate. The combined organic layers were washed with aqueous NaHCO3 (sat.) and brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was used directly for the next step. MS(ISP): 185.21 ([MH]+.
後処理
- additionpoured onto ice water
- extractionThe mixture was extracted twice with ethyl acetate
- washThe combined organic layers were washed with aqueous NaHCO3 (sat.) and brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-62f6afb793ad4b1d9298364b1f73f3fc
- 出典データセット
- uspto-grants-2009_04
- 特許番号
- US07524823B2
反応ノート
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