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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
ノート
印刷プレビュー

反応式

HRID 617130 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 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)-

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-868fe2344e1946bfabbf3ff10befefe9
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05948775

反応ノート

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