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

HRID 1249744노트

반응식

HRID 1249744 반응식
[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

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 135679869HCID 135679869, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ef359185d5604517834247d5b7313891
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06335344B1

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