Phosphorus oxychloride → 4-Chloro-5-iodo-alpha,alpha,alpha-trifluoro-2-picoline
反応式
[I:1][C:2]1[C:3](O)=[CH:4][C:5]([C:8]([F:11])([F:10])[F:9])=[N:6][CH:7]=1.O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:3]1[C:2]([I:1])=[CH:7][N:6]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:4]=1参加物
3
実験手順
A solution of 5-iodo-2-(trifluoromethyl)pyridin-4-ol (4.8 g, 16.6 mmol) in POCl3 (30 mL) was heated to 100° C. for 30 minutes. The resulting solution was concentrated under vacuum and the residue was neutralized by the addition of ice and aqueous potassium carbonate. The solution was extracted with ethyl acetate, dried (Na2SO4), filtered and concentrated under vacuum to give 4-chloro-5-iodo-2-(trifluoromethyl)pyridine. Retention time (min)=2.594, method [1], MS(ESI) 307.9 (M+H).
後処理
- concentrationThe resulting solution was concentrated under vacuum
- additionthe residue was neutralized by the addition of ice and aqueous potassium carbonate
- extractionThe solution was extracted with ethyl acetate
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-9823bd31297c4e079e6f80b2e97a58a5
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09073891B2
反応ノート
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