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

HRID 27901

反応式

HRID 27901 の反応式
[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

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 778863,5-Dichloro-3-pyridylamineHCID 178418790HCID 178418790、化合物

生成物 1

HCID 233404453,5-Dichloro-2-isothiocyanatopyridine

実験手順

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°.

後処理

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

出典と根拠

ORDレコード
ord-dffacfefda164193be659bca22101673
出典データセット
uspto-grants-1980_09
特許番号
US04224331

関連ノート

読み込み中…