Potassium Hydroxide → Boc-D-Glu-OH

HRID 1871208ノート

反応式

HRID 1871208 の反応式
[NH2:1][C@@H:2]([C:8]([OH:10])=[O:9])[CH2:3][CH2:4][C:5](=[O:7])[OH:6].[OH-].[K+].[O:13](C(OC(C)(C)C)=O)[C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=O>O.O1CCOCC1>[NH:1]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:13])[C@@H:2]([C:8]([OH:10])=[O:9])[CH2:3][CH2:4][C:5](=[O:6])[OH:7]

参加物

6

反応物 3

HCID 14797Potassium HydroxideHCID 23327D-Glutamic AcidHCID 90495Di-tert-butyl dicarbonate

生成物 1

HCID 7019046Boc-D-Glu-OH

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

14.7 g (0.1 Mol) of H-D-Glu-OH was dissolved in 200 ml of distilled water, and the pH was adjusted to 10.2 with 0.1M potassium hydroxide. 33.0 g (0.3 Mol) of BOC2O in dioxane was added with intensive mixing. The pH was controlled using a pH-stat. After completion of the reaction, the mixture was transferred to a separating funnel, and extraction was carried out from the alkaline solution with ethyl acetate (3×150 ml). The pH of the aqueous phase was adjusted to 3.0 using 0.2% sulphuric acid, and Boc-D-Glu-OH was extracted from the organic phase (3×200 ml). The organic phase was washed three times with 200 ml of Na2SO4 saturated solution to neutral pH, and dried over Na2SO4, and evaporated to oil under vacuum. The yield was 16.7 g (68%).

後処理

  1. customAfter completion of the reaction
  2. customthe mixture was transferred to a separating funnel
  3. extractionextraction
  4. extractionwas extracted from the organic phase (3×200 ml)
  5. washThe organic phase was washed three times with 200 ml of Na2SO4 saturated solution to neutral pH
  6. dry with materialdried over Na2SO4
  7. customevaporated to oil under vacuum

出典と根拠

ORDレコード
ord-e7a16e7f14cf4e7fb80a2c8eadc4ccf9
出典データセット
uspto-grants-2000_08
特許番号
US06103699

反応ノート

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