Ethyl Acetate → HCID 178440080、化合物

HRID 53031ノート

反応式

HRID 53031 の反応式
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]

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 87885Chloromethyl pivalateHCID 178440085HCID 178440085、化合物

生成物 1

HCID 178440080HCID 178440080、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b2166487533d4bce9cfce82d0809634a
出典データセット
uspto-grants-1997_04
特許番号
US05616599

反応ノート

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