Hydrochloric Acid → 3,5-Dichloro-2-isothiocyanatopyridine

반응식

[Cl:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.Cl.[N-]=[C:12]=[S:13]>>[Cl:1][C:2]1[C:3]([N:9]=[C:12]=[S:13])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1

참가 물질

반응물 3

HCID 313Hydrochloric Acid

HCID 778863,5-Dichloro-3-pyridylamine

HCID 178418790HCID 178418790, 화합물

생성물 1

HCID 233404453,5-Dichloro-2-isothiocyanatopyridine

실험 절차

3,5-Dichloro-2-amino pyridine (8.15, 0.05 mol) was treated with thiophosgenes (10% soln. in toluene, 55 ml). The mixture was refluxed until clear solution was obtained and no further hydrochloric acid gas was being evolved. The mixture was cooled, and the solid which crystallised was removed by filtration. The mother liquors, after evaporation and crystallisation of the residual oil, yielded 5.5 g. (55%) of the required isothiocyanate as pale yellow needles m. pt. 45°-6°.

후처리

temperatureThe mixture was refluxed until clear solution
customwas obtained
temperatureThe mixture was cooled
customthe solid which crystallised
customwas removed by filtration
customThe mother liquors, after evaporation and crystallisation of the residual oil
customyielded 5.5 g

출처 및 근거

ORD 기록: ord-dffacfefda164193be659bca22101673
출처 데이터셋: uspto-grants-1980_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04224331

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