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Benzaldehyde → 1-isopropyl-4-phenyl-3,4,6,7-tetrahydro-furo[3,2-g] quinazolin-2(1H)-one

HRID 1658287
ノート
印刷プレビュー

反応式

HRID 1658287 の反応式
[CH:1]([N:4]([C:8]1[CH:16]=[CH:15][C:11]2[CH2:12][CH2:13][O:14][C:10]=2[CH:9]=1)[C:5]([NH2:7])=[O:6])([CH3:3])[CH3:2].[CH:17](=O)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CS(O)(=O)=O.C1(C)C=CC=CC=1>[CH:1]([N:4]1[C:8]2[C:16](=[CH:15][C:11]3[CH2:12][CH2:13][O:14][C:10]=3[CH:9]=2)[CH:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[NH:7][C:5]1=[O:6])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 240BenzaldehydeHCID 21528985N-(2,3-Dihydro-1-benzofuran-6-yl)-N-propan-2-ylurea

生成物 1

HCID 215289561-isopropyl-4-phenyl-3,4,6,7-tetrahydro-furo[3,2-g] quinazolin-2(1H)-one

試薬・触媒・溶媒 2

HCID 6395Methanesulfonic Acid触媒HCID 1140Toluene溶媒

実験手順

A solution of 8.0 g. of 1-Isopropyl-1-(2,3-dihydro-6-benzofuranyl)urea, 3.6 ml. of benzaldehyde, 5 drops of methanesulfonic acid and 200 ml. of toluene is stirred and refluxed under a water separator for 20 hours. The resulting solution is cooled and the cooled solution is washed twice with 150 ml. water, dried with anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue is dissolved in a minimum amount of chloroform and chromatographed on silica gel (200 g.) using chloroform as an eluent to give an oil of 1-isopropyl-4-phenyl-3,4,6,7-tetrahydro-furo[3,2-g] quinazolin-2(1H)-one and an oil of 6-isopropyl -9-phenyl-2,3,8,9-tetrahydro-furan[2,3-f]quinazolin-7(6H)-one.

後処理

  1. temperaturerefluxed under a water separator for 20 hours
  2. temperatureThe resulting solution is cooled
  3. washthe cooled solution is washed twice with 150 ml
  4. dry with materialwater, dried with anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. dissolutionThe residue is dissolved in a minimum amount of chloroform
  8. customchromatographed on silica gel (200 g.)

出典と根拠

ORDレコード
ord-8f0bc856b5074eeabfd39323e8bef263
出典データセット
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03963717

反応ノート

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