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1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 23060629、化合物

HRID 750362
ノート
印刷プレビュー

反応式

HRID 750362 の反応式
[C:1]([C:9]1[CH:34]=[C:33]([Br:35])[CH:32]=[CH:31][C:10]=1[C:11]([N:13]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([S:27]([CH3:30])(=[O:29])=[O:28])=[CH:23][CH:22]=1)[CH2:14][C:15](=[O:19])[CH2:16][CH2:17][CH3:18])=[O:12])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N12CCCN=C1CCCCC2>C1(C)C=CC=CC=1>[Br:35][C:33]1[CH:34]=[C:9]2[C:10](=[CH:31][CH:32]=1)[C:11](=[O:12])[N:13]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([S:27]([CH3:30])(=[O:29])=[O:28])=[CH:23][CH:22]=1)[C:14]([C:15](=[O:19])[CH2:16][CH2:17][CH3:18])=[C:1]2[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 230608192-benzoyl-4-bromo-N-(4-methanesulfonylbenzyl)-N-(2-oxopentyl)benzamide

生成物 1

HCID 23060629HCID 23060629、化合物収率 72.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

[Step 3] To a solution (40 ml) of 2-benzoyl-4-bromo-N-(4-methanesulfonylbenzyl)-N-(2-oxopentyl)benzamide (2.0 g) in toluene was added 1,8-diazabicyclo[5.4.0]undeca-7-ene (1.1 g), and the mixture was heated under reflux for 48 hrs. The reaction mixture was concentrated under reduced pressure. To the residue were added water and 10% hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, saturated aqueous sodium hydrogen carbonate, water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by recrystallization (THF-diisopropyl ether) to give the title compound (1.4 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 48 hrs
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionTo the residue were added water and 10% hydrochloric acid
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with water, saturated aqueous sodium hydrogen carbonate, water and saturated brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customthe residue was purified by recrystallization (THF-diisopropyl ether)

出典と根拠

ORDレコード
ord-3313ca07526c4cf0adf540abbac8e236
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07402595B2

反応ノート

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