Phosphorus oxychloride → 2-chloro-3-phenylpyrazine

반응식

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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 1559662-Hydroxy-3-phenylpyrazine

생성물 1

HCID 8246672-chloro-3-phenylpyrazine

실험 절차

A 0.01 mol. sample of 3-phenylpyrazin-2(1H)one is mixed with 9.0 ml. of phosphorous oxychloride (POCl3) and refluxed for 5-6 hr. The excess phosphorous oxychloride is removed by distillation at reduced pressure and 25 ml. of methylene chloride added to the residue. The resultant solution is stirred with a few milliliters of ice water, dried, evaporated and the residue recrystallized to yield the title compound.

후처리

customThe excess phosphorous oxychloride is removed by distillation at reduced pressure and 25 ml
additionof methylene chloride added to the residue
customdried
customevaporated
customthe residue recrystallized

출처 및 근거

ORD 기록: ord-370af20a5193473586928eff3cc9b7e5
출처 데이터셋: uspto-grants-1983_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04402958

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