Sulfuric Acid → D-Valine, 3-(methylthio)-

HRID 324285

反応式

HRID 324285 の反応式
[NH2:1][C@@H:2]([C:7]([OH:9])=[O:8])[C:3]([SH:6])([CH3:5])[CH3:4].O.O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-].S(OC)(O[CH3:25])(=O)=O.S(=O)(=O)(O)O>>[CH3:25][S:6][C:3]([CH3:5])([CH3:4])[C@H:2]([C:7]([OH:9])=[O:8])[NH2:1]

参加物

5

反応物 4

HCID 1118Sulfuric AcidHCID 5852PenicillamineHCID 6497Dimethyl SulfateHCID 17749109Barium hydroxide, octahydrate

生成物 1

HCID 10329618D-Valine, 3-(methylthio)-収率 100%

実験手順

A suspension of D-Penicillamine (10.0 g, 67.01 mmol) in 0.4N solution of barium hydroxide octahydrate (330 mL, 67.01 mmol) is chilled on an ice water bath. Dimethyl sulfate (6.6 mL, 70.36 mmol, 1.05 equiv) is added dropwise over a period of 30 minutes. The suspension stirred for 18 hours at room temperature. A solution of 1 N sulfuric acid is added to the solution (pH˜2) to precipitate out the barium sulfate. The supernatent is decanted and the precipitate is washed several times with water. The pH of the supernatent is adjusted to 6 with concentrated ammonium hydroxide and the water is evaporated off to give a pure white solid (10.9 g, 100% yield).

後処理

  1. temperatureis chilled on an ice water bath
  2. customto precipitate out the barium sulfate
  3. customThe supernatent is decanted
  4. washthe precipitate is washed several times with water
  5. customthe water is evaporated off

出典と根拠

ORDレコード
ord-04336a88bb094f4c96b11adc5567f5c6
出典データセット
uspto-grants-2001_04
特許番号
US06218389B1

関連ノート

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