Bromoform → Methyl 2-bromothiazole-5-carboxylate

반응식

[N+]([O-])(OCCCCC)=O.[CH:10]([Br:13])(Br)Br.NC1[S:16][C:17]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][N:19]=1>>[Br:13][C:10]1[S:16][C:17]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][N:19]=1

참가 물질

반응물 3

HCID 5558Bromoform

HCID 61250Amyl Nitrate

HCID 238005Methyl 2-aminothiazole-5-carboxylate

생성물 1

HCID 2773502Methyl 2-bromothiazole-5-carboxylate

실험 절차

A mixture containing 100 g. of amyl nitrate and 600 ml. of bromoform is warmed to 70° C and then a total of 100 g. of 2-amino-5-methoxycarbonylthiazole is added portionwise with rapid stirring while maintaining the temperature at about 95°-100° C. The mixture is then stirred for an additional ten minutes at this temperature and then the bromoform is distilled off under vacuum. The residue is chromatographed on silica gel yielding 2-bromo-5-methoxycarbonylthiazole.

후처리

additionA mixture containing 100 g
temperaturewhile maintaining the temperature at about 95°-100° C
stirringThe mixture is then stirred for an additional ten minutes at this temperature
distillationthe bromoform is distilled off under vacuum
customThe residue is chromatographed on silica gel

출처 및 근거

ORD 기록: ord-f18bc3313aa14100afdb4d913b8f62e3
출처 데이터셋: uspto-grants-1978_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04089865

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