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Acetone → HCID 178440097, 화합물

HRID 53033
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HRID 53033 반응식
[BH4-].[Na+].[C:3]([C:6]1[N:7]=[C:8]([CH2:16][CH2:17][CH3:18])[NH:9][C:10]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])(=[O:5])[CH3:4].CC(C)=O>C(O)C>[OH:5][CH:3]([C:6]1[N:7]=[C:8]([CH2:16][CH2:17][CH3:18])[NH:9][C:10]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 180AcetoneHCID 4311764Sodium borohydrideHCID 10513320ethyl 4-acetyl-2-propyl-1H-imidazole-5-carboxylate

생성물 1

HCID 178440097HCID 178440097, 화합물수율 87.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

125 mg of sodium borohydride were added to a solution of 1.50 g of ethyl 4-acetyl-2-propylimidazole-5-carboxylate [prepared as described in step (ii) above] in 15 ml of ethanol, and the resulting mixture was stirred at room temperature for 30 minutes. 2 ml of acetone were added, and the mixture was stirred for a further 10 minutes. The reaction mixture was then concentrated by evaporation under reduced pressure, and the concentrate was dissolved in methanol. The solution was again concentrated by evaporation under reduced pressure, and the residue was purified by column chromatography through silica gel, using 1:20 and 1:10 by volume mixtures of methylene chloride and methanol as the eluent, to give 1.32 g of the title compound as crystals, melting at 151°-153° C.

후처리

  1. stirringthe mixture was stirred for a further 10 minutes
  2. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure
  3. dissolutionthe concentrate was dissolved in methanol
  4. concentrationThe solution was again concentrated by evaporation under reduced pressure
  5. customthe residue was purified by column chromatography through silica gel

출처 및 근거

ORD 기록
ord-f722cfd71cc94e1aa106548e3474c1f3
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05616599

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