3,4-dihydro-2H-pyran → HCID 19969552、化合物

HRID 974859ノート

反応式

HRID 974859 の反応式
O.C1(C)C(S(O)(=O)=O)=CC=CC=1.[CH2:13]([O:15][C:16]([CH:18]1[NH:23][C:22](=[O:24])[CH:21]([CH2:25][CH:26]([CH3:28])[CH3:27])[N:20]([OH:29])[C:19]1=[O:30])=[O:17])[CH3:14].[O:31]1[CH:36]=[CH:35][CH2:34][CH2:33][CH2:32]1>ClCCl>[CH2:13]([O:15][C:16]([CH:18]1[NH:23][C:22](=[O:24])[CH:21]([CH2:25][CH:26]([CH3:27])[CH3:28])[N:20]([O:29][CH:32]2[CH2:33][CH2:34][CH2:35][CH2:36][O:31]2)[C:19]1=[O:30])=[O:17])[CH3:14]

参加物

5

反応物 3

HCID 80803,4-dihydro-2H-pyranHCID 124969952-Methylbenzenesulfonic acid hydrateHCID 19969538HCID 19969538、化合物

生成物 1

HCID 19969552HCID 19969552、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.45 g of p, toluenesulfonic acid hydrate was added to 60 ml of a solution of 6.15 g of 3-ethoxycarbonyl-1-hydroxy-6-isobutylpiperazine-2,5-dione and 4 ml of 3,4-dihydro-2H-pyran in anhydrous dichloromethane. The mixture was stirred at room temperature for 4 hours. The reaction mixture was washed with an aqueous solution saturated with sodium hydrogen carbonate and then dried with anhydrous magnesium sulfate. The resulting mixture was subjected to distillation to remove the solvent to obtain 9.67 g of 3-ethoxycarbonyl-6-isobutyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione as an orange oily substance.

後処理

  1. washThe reaction mixture was washed with an aqueous solution saturated with sodium hydrogen carbonate
  2. dry with materialdried with anhydrous magnesium sulfate
  3. distillationThe resulting mixture was subjected to distillation
  4. customto remove the solvent

出典と根拠

ORDレコード
ord-2ab6faded25340c787eb799c4fb870e9
出典データセット
uspto-grants-1997_03
特許番号
US05607934

反応ノート

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