Phosphorus oxychloride → 4-Chloro-6-phenylpyrimidine

반응식

O[C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[CH:4][N:3]=1.P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[CH:4][N:3]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178515560HCID 178515560, 화합물

생성물 1

HCID 5934294-Chloro-6-phenylpyrimidine수율 93.5%

실험 절차

Crude 4-hydroxy-6-phenylpyrimidine (3.65 g) was heated to reflux with phosphoryl chloride (40 ml) for 90 minutes. The reaction mixture was cooled and then concentrated under reduced pressure to afford a brown solid. The brown solid was partitioned between water and ether and the combined ether extracts washed with brine, dried and evaporated to give 4-chloro-6-phenylpyrimidine (2.18 g, 93.5% pure by GC analysis) as a yellow solid which was used directly in the next stage.

후처리

temperatureThe reaction mixture was cooled
concentrationconcentrated under reduced pressure
customto afford a brown solid
customThe brown solid was partitioned between water and ether
washthe combined ether extracts washed with brine
customdried
customevaporated

출처 및 근거

ORD 기록: ord-5c9af44dc84d48af91e26c2dbc3c421d
출처 데이터셋: uspto-grants-2003_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06613773B2

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