D-Leucine → (R)-2-hydroxy-4-methylpentanoic acid

HRID 1464367

反応式

HRID 1464367 の反応式
N[C@@H:2]([C:7]([OH:9])=[O:8])[CH2:3][CH:4]([CH3:6])[CH3:5].N([O-])=[O:11].[Na+]>O.S(=O)(=O)(O)O>[C:7]([OH:9])(=[O:8])[C@@H:2]([CH2:3][CH:4]([CH3:6])[CH3:5])[OH:11]

参加物

5

反応物 2

HCID 439524D-LeucineHCID 23668193Sodium Nitrite

生成物 1

HCID 439960(R)-2-hydroxy-4-methylpentanoic acid収率 41.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 1118Sulfuric Acid溶媒

実験手順

400 g of D-leucine was dissolved in 5 l of water containing 296 ml of concentrated sulfuric acid and cooled to -2°. A solution of 421 g of sodium nitrite in 1.25 l of water was added slowly while holding the temperature at -2°. The mixture was stirred at 0° for 1.5 hours and then allowed to warm to room temperature overnight. The mixture was extracted three times with ethyl acetate. The combined organic extracts were washed with sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated to give 168 g of D-leucic acid as a pale yellow oil.

後処理

  1. temperaturecooled to -2°
  2. customat -2°
  3. extractionThe mixture was extracted three times with ethyl acetate
  4. washThe combined organic extracts were washed with sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated

出典と根拠

ORDレコード
ord-69c19abdbb464d54854f17c34badf796
出典データセット
uspto-grants-1994_04
特許番号
US05304549

関連ノート

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