Phosphorus tribromide → 4-Bromo-2-(trifluoromethyl)pyrimidine

반응식

[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[C:7](O)[CH:6]=[CH:5][N:4]=1.P(Br)(Br)[Br:13]>>[Br:13][C:7]1[CH:6]=[CH:5][N:4]=[C:3]([C:2]([F:11])([F:10])[F:1])[N:8]=1

참가 물질

반응물 2

HCID 24614Phosphorus tribromide

HCID 178516506HCID 178516506, 화합물

생성물 1

HCID 533023444-Bromo-2-(trifluoromethyl)pyrimidine

반응 조건

온도: 150 °C

실험 절차

The 2-(trifluoromethyl)pyrimidin-4-ol (328 mg, 2.0 mmol) and PBr3 (0.188 mL, 2.0 mmol) were mixed and heated at 150° C. for 3 h. The reaction was cooled down and quenched with ice water, extracted with DCM (20 mL×2) to yield the titled compound. The organic phase was concentrated and crude material was purified by preparative TLC with 20% Acetone:Hexane to yield titled compound.

후처리

temperatureThe reaction was cooled down
customquenched with ice water
extractionextracted with DCM (20 mL×2)

출처 및 근거

ORD 기록: ord-bcec6bd2fc714ad48b39e26ebfcac891
출처 데이터셋: uspto-grants-2013_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08445499B2

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