Hydrochloric Acid → HCID 19969579, 화합물

HRID 974858노트

반응식

HRID 974858 반응식
[OH-].[Na+].[CH2:3]([C:10]1([C:30]([O:32]CC)=[O:31])[NH:15][C:14](=[O:16])[CH:13]([CH2:17][CH:18]([CH3:20])[CH3:19])[N:12]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:11]1=[O:29])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl.C(OCC)(=O)C>C(O)C.O>[CH2:3]([C:10]1([C:30]([OH:32])=[O:31])[NH:15][C:14](=[O:16])[CH:13]([CH2:17][CH:18]([CH3:20])[CH3:19])[N:12]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:11]1=[O:29])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 19969576HCID 19969576, 화합물

생성물 1

HCID 19969579HCID 19969579, 화합물수율 99.9%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

5.3 ml of 1N sodium hydroxide was added to 25 ml of a suspension of 2.32 g of (3RS,6SR)-3-benzyl-1-benzyloxy-3-ethoxycarbonyl-6-isobutylpiperazine-2,5-dione in ethanol. The mixture was stirred at room temperature for 1.5 hours. The reaction mixture was adjusted to pH 3 with 1N hydrochloric acid. Thereto were added 80 ml of ethyl acetate and 80 ml of water to conduct distribution. The organic layer was dried with anhydrous magnesium sulfate and then subjected to vacuum distillation to remove the solvent at room temperature to obtain 2.17 g of (3RS,6SR)-3-benzyl-1-benzyloxy-3-carboxy-6-isobutylpiperazine-2,5-dione as a light yellow solid.

후처리

  1. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  2. distillationsubjected to vacuum distillation
  3. customto remove the solvent at room temperature

출처 및 근거

ORD 기록
ord-ea1d3949ab4e4f37804955cad419a35d
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607934

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