Ethyl Acetate → HCID 178440076, 화합물

HRID 53038

반응식

HRID 53038 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].[CH3:25][C:26]1[O:30][C:29](=[O:31])[O:28][C:27]=1[CH2:32]Cl.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][C:27]1[O:28][C:29](=[O:31])[O:30][C:26]=1[CH3:25])=[O:20])([CH3:13])[CH3:12]

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 98555184-(Chloromethyl)-5-methyl-1,3-dioxol-2-oneHCID 178440085HCID 178440085, 화합물

생성물 1

HCID 178440076HCID 178440076, 화합물수율 70.4%

시약·촉매·용매 2

HCID 962Water용매HCID 31374Dimethylacetamide용매

실험 절차

1.76 ml of N,N-diisopropylethylamine were added to a suspension of 1.06 g of 4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylic acid [prepared as described in Preparation 22(i)] in 10 ml of N,N-dimethylacetamide, and the resulting mixture was stirred at room temperature for 10 minutes, after which 1.12 g of (5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl chloride was added, and the mixture was stirred at 60° C. for 4 hours. At the end of this time, the reaction mixture was mixed with ethyl acetate and water. The ethyl acetate layer was separated and concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 1:15 by volume mixture of methanol and methylene chloride as the eluent, to give 1.14 g of the title compound as a viscous oil.

후처리

  1. stirringthe 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 concentrate was purified by column chromatography through silica gel
  5. additionby volume mixture of methanol and methylene chloride as the eluent

출처 및 근거

ORD 기록
ord-77263688991d49449e335cb5d66ac1fd
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616599

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