Phosphorus oxychloride → 2-Chloro-4-phenylthiazole

반응식

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

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178517449HCID 178517449, 화합물

생성물 1

HCID 27613592-Chloro-4-phenylthiazole수율 65.2%

실험 절차

A mixed solution of 4-phenyl-1,3-thiazol-2-ol (2.00 g, 11.3 mmol) in phosphorus oxychloride (20 ml) was stirred at 100° C. for 2 hours. The solvent was distilled off under reduced pressure. The residue was poured to ice water and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to give 1.44 g (65.2%) of the desired product as a solid.

후처리

distillationThe solvent was distilled off under reduced pressure
additionThe residue was poured to ice water
extractionextracted with ethyl acetate
washThe extract was washed with water
dry with materialdried over anhydrous magnesium sulfate
distillationThe solvent was distilled off under reduced pressure
customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)

출처 및 근거

ORD 기록: ord-41fa803d4b4941b2aba444587b98589a
출처 데이터셋: uspto-grants-2010_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07851473B2

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