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Hydrochloric Acid → 6-benzoyl-3,4-dihydro-2(1H)-quinazolinone

HRID 2247886
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HRID 2247886 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[NH:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH2:17][NH:16][C:15]1=[O:24].Cl>CN(C)C=O>[C:5]([C:20]1[CH:19]=[C:18]2[C:23](=[CH:22][CH:21]=1)[NH:14][C:15](=[O:24])[NH:16][CH2:17]2)(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7412Benzoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 123607561,2,3,4-Tetrahydroquinazolin-2-one

생성물 1

HCID 198160376-benzoyl-3,4-dihydro-2(1H)-quinazolinone수율 76.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

반응 조건

온도
70 °C

실험 절차

To a vigorously stirred amount of 45 parts of aluminum chloride were added dropwise 7.05 parts of N,N-dimethylformamide. After stirring for 5 min. at 70° C., there were added 5 parts of benzoyl chloride and, dropwise, 4.7 parts of 3,4-dihydro-2(1H)-quinazolinone. Stirring was continued for 2 hours at 70° C. The reaction mixture was poured into ice-water and there were added 63.5 parts of HCl. The precipitate was filtered off and recrystallized from 2-methoxyethanol, yielding 6.5 parts (76.4%) of 6-benzoyl-3,4-dihydro-2(1H)-quinazolinone; mp. 264.8° C. (interm. 1).

후처리

  1. stirringStirring
  2. waitwas continued for 2 hours at 70° C
  3. filtrationThe precipitate was filtered off
  4. customrecrystallized from 2-methoxyethanol

출처 및 근거

ORD 기록
ord-38053b881e014e169f8a5f7fcffe0981
출처 데이터셋
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05037829

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