Phosphorus oxychloride → 2-Chloro-5-phenyloxazole

HRID 613984ノート

反応式

HRID 613984 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 109976262-Chloro-5-phenyloxazole

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ff4aa09c23e1459388d2253bd77629ad
出典データセット
uspto-grants-1979_03
特許番号
US04143047

反応ノート

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