Hydrochloric Acid → HCID 18604408、化合物

HRID 1010911ノート

反応式

HRID 1010911 の反応式
[NH:1]1[CH2:8][CH2:7][CH2:6][C@@:2]1([CH3:9])[C:3]([OH:5])=[O:4].Cl[C:11]([O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:12].[OH-].[Na+].Cl>O1CCOCC1.O>[CH2:14]([O:13][C:11]([N:1]1[CH2:8][CH2:7][CH2:6][C@@:2]1([CH3:9])[C:3]([OH:5])=[O:4])=[O:12])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 10387Benzyl chloroformateHCID 14798Sodium HydroxideHCID 69936642-Methyl-L-proline

生成物 1

HCID 18604408HCID 18604408、化合物収率 82.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To the solution prepared by dissolving 500 mg of H-α-Me-Pro-OH (commercially available from Chem-Impex International Inc.) and 693 mg of benzyl chloroformate in 10 mL of 1,4-dioxane and 5 mL of water, a 1 M aqueous sodium hydroxide solution was added at room temperature so as to keep pH 10, and the solution was stirred at room temperature for 30 minutes. To the reaction solution, 5 M HCl was added so as to adjust the pH to 2, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The insolubles were filtered, and the filtrate was concentrated under reduced pressure to obtain 842 mg of 1-[(benzyloxy)carbonyl]-2-methyl-L-proline [63-1] (hereinafter, referred to as the compound [63-1]).

後処理

  1. customTo the solution prepared
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe obtained organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe insolubles were filtered
  6. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-a623d564fe394a9eb9a70207f9de0700
出典データセット
uspto-grants-2011_07
特許番号
US07977336B2

反応ノート

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