3,4-dihydro-2H-pyran → HCID 19969552, 화합물

HRID 974859노트

반응식

HRID 974859 반응식
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]

참가 물질

5

반응물 3

HCID 80803,4-dihydro-2H-pyranHCID 124969952-Methylbenzenesulfonic acid hydrateHCID 19969538HCID 19969538, 화합물

생성물 1

HCID 19969552HCID 19969552, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2ab6faded25340c787eb799c4fb870e9
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607934

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