2-Butyl-6-(1-hydroxyethyl)-3-[[2'-[1-(triphenylmethyl)-1H-tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-4(3H)-quinazolinone → HCID 178441465、化合物

HRID 486031ノート

反応式

HRID 486031 の反応式
[CH2:1]([C:5]1[N:14]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:28]3[N:32](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:31]=[N:30][N:29]=3)=[CH:18][CH:17]=2)[C:13](=[O:52])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([CH:53]([OH:55])[CH3:54])[CH:11]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4]>CC(C)=O.O.Cl>[CH2:1]([C:5]1[N:14]([CH2:15][C:16]2[CH:17]=[CH:18][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[C:28]3[NH:29][N:30]=[N:31][N:32]=3)=[CH:20][CH:21]=2)[C:13](=[O:52])[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([CH:53]([OH:55])[CH3:54])[CH:11]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 1

HCID 200793502-Butyl-6-(1-hydroxyethyl)-3-[[2'-[1-(triphenylmethyl)-1H-tetrazol-5-yl][1,1'-biphenyl]-4-yl]methyl]-4(3H)-quinazolinone

生成物 1

HCID 178441465HCID 178441465、化合物収率 68.8%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 18366337Propan-2-one--water (1/1)溶媒

実験手順

To a suspension of 2.00 g of 2-butyl-6-(1-hydroxyethyl)-3-[[2'-[1-(triphenylmethyl)-1H-tetrazol-5-yl][1,1'biphenyl]-4-yl]methyl]-4(3H)-quinazolinone in 70 ml of 3:1 acetone-water is added one drop of 5% aqueous hydrochloric acid solution. The mixture is then heated at reflux for 16 hours. After cooling, the reaction mixture is concentrated in vacuo and the residue purified by flash chromatography on silica gel by elution with 9:1 chloroform-methanol to afford 0.915 g of the desired product as a white solid, m.p. 146°-147° C.

後処理

  1. temperatureThe mixture is then heated
  2. temperatureat reflux for 16 hours
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture is concentrated in vacuo
  5. customthe residue purified by flash chromatography on silica gel by elution with 9:1 chloroform-methanol

出典と根拠

ORDレコード
ord-09b42366cc4f4003bf58f08c836eaad2
出典データセット
uspto-grants-1994_03
特許番号
US05290780

反応ノート

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