Water → HCID 178441858、化合物

HRID 1975446ノート

反応式

HRID 1975446 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([C:11]1[NH:12][C:13]2[C:18]([C:19](=[O:21])[N:20]=1)=[CH:17][C:16]([C:22](OC)=[O:23])=[CH:15][CH:14]=2)[CH2:8][CH2:9][CH3:10].O>O1CCCC1>[CH2:7]([C:11]1[NH:12][C:13]2[C:18]([C:19](=[O:21])[N:20]=1)=[CH:17][C:16]([CH2:22][OH:23])=[CH:15][CH:14]=2)[CH2:8][CH2:9][CH3:10]

参加物

5

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydride3 回HCID 178441861methyl 2-butyl-4-oxo-1H-quinazoline-6-carboxylate

生成物 1

HCID 178441858HCID 178441858、化合物収率 44.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of 0.013 g of lithium aluminum hydride in 5.0 ml of tetrahydrofuran is added 0.100 g of methyl 2-butyl-1,4-dihydro-4-oxo-6-quinazolinecarboxylate followed by stirring at room temperature for 5 hours. An additional 20 mg of lithium aluminum hydride is added and stirring continued for 18 hours. An additional 20 mg of lithium aluminum hydride is added and stirring continued for an additional 8 hours. The reaction mixture is poured into 75 ml of water and extracted with ethyl acetate. The extract is evaporated in vauco to a residue which is stirred with acetone and filtered to give 0.040 g of the desired product as a white solid.

後処理

  1. stirringstirring
  2. waitcontinued for 18 hours
  3. stirringstirring
  4. waitcontinued for an additional 8 hours
  5. extractionextracted with ethyl acetate
  6. customThe extract is evaporated in vauco to a residue which
  7. stirringis stirred with acetone
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-32cfab9d3905401e8378159d82d0135a
出典データセット
uspto-grants-1994_02
特許番号
US05286729

反応ノート

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