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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 4(3h)-Quinazolinone,2-[4-(2-chloroethoxy)phenyl]-8-methoxy-3-(4-methoxyphenyl)-

HRID 617130
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HRID 617130 반응식
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]2[N:20]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=3)[C:19](=[O:29])[C:18]3[C:13](=[C:14]([O:30][CH3:31])[CH:15]=[CH:16][CH:17]=3)[NH:12]2)=[CH:7][CH:6]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C1(C)C=CC=CC=1>[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[N:20]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=3)[C:19](=[O:29])[C:18]3[C:13](=[C:14]([O:30][CH3:31])[CH:15]=[CH:16][CH:17]=3)[N:12]=2)=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 218510814(1h)-Quinazolinone,2-[4-(2-chloroethoxy)phenyl]-2,3-dihydro-8-methoxy-3-(4-methoxyphenyl)-

생성물 1

HCID 158708824(3h)-Quinazolinone,2-[4-(2-chloroethoxy)phenyl]-8-methoxy-3-(4-methoxyphenyl)-

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 18.0 g (0.0410 mol) of 2-[4-(2-chloro-ethoxy)-phenyl]-8-methoxy-3-(4-methoxy-phenyl)-2,3-dihydro-1H-quinazolin-4-one in 500 mL of toluene was added 9.31 g (0.0410 mol) of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone. The reaction mixture was stirred and heated under reflux for 3 hours. After cooling to room temperature, the solvent was removed in a rotary evaporator. Ethanol (300 mL) was added to the crude product and stirred at room temperature overnight. The precipitate was collected by vacuum filtration. An analytical sample (mp 151-152° C.) was obtained by recrystallization from ethanol.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. customthe solvent was removed in a rotary evaporator
  4. additionEthanol (300 mL) was added to the crude product
  5. stirringstirred at room temperature overnight
  6. filtrationThe precipitate was collected by vacuum filtration
  7. customAn analytical sample (mp 151-152° C.) was obtained by recrystallization from ethanol

출처 및 근거

ORD 기록
ord-868fe2344e1946bfabbf3ff10befefe9
출처 데이터셋
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05948775

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