Hydrochloric Acid → HCID 19969579、化合物

HRID 974858ノート

反応式

HRID 974858 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 19969576HCID 19969576、化合物

生成物 1

HCID 19969579HCID 19969579、化合物収率 99.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ea1d3949ab4e4f37804955cad419a35d
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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