Water → HCID 178441858, 화합물

HRID 1975446노트

반응식

HRID 1975446 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydride3회HCID 178441861methyl 2-butyl-4-oxo-1H-quinazoline-6-carboxylate

생성물 1

HCID 178441858HCID 178441858, 화합물수율 44.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-32cfab9d3905401e8378159d82d0135a
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286729

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