Phosphorus oxychloride → 2-Chloro-4-phenylthiazole

반응식

O[C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:2]1[S:3][CH:4]=[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178517449HCID 178517449, 화합물

생성물 1

HCID 27613592-Chloro-4-phenylthiazole

실험 절차

To 80 ml of phosphorus oxychloride were added 7.7 g (43 mmol) of 2-hydroxy-4-phenylthiazole, followed by heating at 100°-105° C. for 2 hours. The solvent was then distilled off from the reaction mixture under reduced pressure. Ice water was added to the residue, followed by extraction with ethyl ether. The ether layer was washed with water. After purification by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1), the title compound was obtained as pale yellow crystals.

후처리

temperatureby heating at 100°-105° C. for 2 hours
distillationThe solvent was then distilled off from the reaction mixture under reduced pressure
additionIce water was added to the residue
extractionfollowed by extraction with ethyl ether
washThe ether layer was washed with water
customAfter purification by silica gel column chromatography (solvent: hexane/ethyl acetate=5/1)

출처 및 근거

ORD 기록: ord-bbd48428ddad4311a4e64414339d0545
출처 데이터셋: uspto-grants-1992_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05112841

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