Phosphorus pentachloride → 8-Chloro-[1,3]dioxolo[4,5-g]quinazoline

HRID 1249744ノート

反応式

HRID 1249744 の反応式
[O:1]1[C:5]2=[CH:6][C:7]3[C:8](=O)[NH:9][CH:10]=[N:11][C:12]=3[CH:13]=[C:4]2[O:3][CH2:2]1.P(Cl)(Cl)(Cl)(Cl)[Cl:16]>P(Cl)(Cl)(Cl)=O>[Cl:16][C:8]1[C:7]2[CH:6]=[C:5]3[O:1][CH2:2][O:3][C:4]3=[CH:13][C:12]=2[N:11]=[CH:10][N:9]=1

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 135679869HCID 135679869、化合物

生成物 1

HCID 149353678-Chloro-[1,3]dioxolo[4,5-g]quinazoline収率 74%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

A mixture of 7H-[1,3]dioxolo[4,5-g]quinazolin-8-one (0.550 g, 2.78 mmol) and phosphorus pentachloride (0.800 g, 3.84 mmol) in 3 mL phosphorus oxychloride was heated to a gentle reflux for 2.5 hours. Solvent was removed in vacuo, and azeotroped with toluene. Residue was dissolved in ethyl acetate and washed with 5% sodium bicarbonate solution and then filtered, and then solvent was removed in vacuo to give 8-chloro-[1,3]dioxolo[4,5-g]quinazoline (0.400 g, 74%).

後処理

  1. temperaturewas heated to
  2. temperaturea gentle reflux for 2.5 hours
  3. customSolvent was removed in vacuo
  4. customazeotroped with toluene
  5. dissolutionResidue was dissolved in ethyl acetate
  6. washwashed with 5% sodium bicarbonate solution
  7. filtrationfiltered
  8. customsolvent was removed in vacuo

出典と根拠

ORDレコード
ord-ef359185d5604517834247d5b7313891
出典データセット
uspto-grants-2002_01
特許番号
US06335344B1

反応ノート

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