Phosphorus oxychloride → 2-Chloro-5-phenyloxazole

HRID 613984노트

반응식

HRID 613984 반응식
[C:1]1([C:7]2[O:11][C:10](=S)[NH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:15])=O>C(N(CC)CC)C>[Cl:15][C:10]1[O:11][C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[CH:8][N:9]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 122308765-Phenyl-1,3-oxazole-2-thiol

생성물 1

HCID 109976262-Chloro-5-phenyloxazole

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

5-Phenyl-2(3H)-oxazolethione (Acta. Chem. Scand. 23 2879 (1969)) (19.6 g, 0.11 m) and phosphorous oxychloride (70 ml) were stirred with cooling during the cautious addition of triethylamine (12.4 g, 0.123 m). The mixture was then heated under reflux for 20 hours, excess reagents removed under reduced pressure and the residue distilled in vacuo to give the title product as a colourless oil which solidified on standing, b.p. 96°-8° C/0.6 mm, m.p. 34° C.

후처리

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux for 20 hours
  3. customexcess reagents removed under reduced pressure
  4. distillationthe residue distilled in vacuo

출처 및 근거

ORD 기록
ord-ff4aa09c23e1459388d2253bd77629ad
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04143047

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