Ethyl Acetate → HCID 178440080, 화합물

HRID 53031

반응식

HRID 53031 반응식
C(N(CC)C(C)C)(C)C.[OH:10][C:11]([C:14]1[N:15]=[C:16]([CH2:22][CH2:23][CH3:24])[NH:17][C:18]=1[C:19]([OH:21])=[O:20])([CH3:13])[CH3:12].[C:25]([O:31][CH2:32]Cl)(=[O:30])[C:26]([CH3:29])([CH3:28])[CH3:27].C(OCC)(=O)C>CN(C)C(=O)C.O>[OH:10][C:11]([C:14]1[N:15]=[C:16]([CH2:22][CH2:23][CH3:24])[NH:17][C:18]=1[C:19]([O:21][CH2:32][O:31][C:25](=[O:30])[C:26]([CH3:29])([CH3:28])[CH3:27])=[O:20])([CH3:13])[CH3:12]

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 87885Chloromethyl pivalateHCID 178440085HCID 178440085, 화합물

생성물 1

HCID 178440080HCID 178440080, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 31374Dimethylacetamide용매

실험 절차

1.76 ml of N,N-diisopropylethylamine were added to a suspension of 1.14 g of 4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylic acid [prepared as described in step (i) above] in 12 ml of N,N-dimethylacetamide, and the resulting mixture was stirred at room temperature for 10 minutes; 1.36 ml of pivaloyloxymethyl chloride was then added. The reaction mixture was stirred at 60° C. for 4 hours, after which it was mixed with ethyl acetate and water. The ethyl acetate layer was separated and concentrated by evaporation under reduced pressure. The crystals which precipitated were triturated with diisopropyl ether and collected by filtration to give 1.53 g of the title compound, melting at 177° C.

후처리

  1. stirringThe reaction mixture was stirred at 60° C. for 4 hours
  2. customThe ethyl acetate layer was separated
  3. concentrationconcentrated by evaporation under reduced pressure
  4. customThe crystals which precipitated
  5. customwere triturated with diisopropyl ether
  6. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-b2166487533d4bce9cfce82d0809634a
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616599

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