Phosphorus oxychloride → 4-Chloro-5-iodo-alpha,alpha,alpha-trifluoro-2-picoline

반응식

[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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178516139HCID 178516139, 화합물

생성물 1

HCID 687560594-Chloro-5-iodo-alpha,alpha,alpha-trifluoro-2-picoline

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록: ord-9823bd31297c4e079e6f80b2e97a58a5
출처 데이터셋: uspto-grants-2015_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09073891B2

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