3-Hydroxy-3-methylglutaric acid monoamide, ammonium salt → 3-Hydroxy-3-methylglutaric acid monoamide

HRID 1706596ノート

反応式

HRID 1706596 の反応式
[NH4+].[OH:2][C:3]([CH3:12])([CH2:8][C:9]([O-:11])=[O:10])[CH2:4][C:5]([NH2:7])=[O:6]>O>[OH:2][C:3]([CH3:12])([CH2:8][C:9]([OH:11])=[O:10])[CH2:4][C:5]([NH2:7])=[O:6]

参加物

3

実験手順

1.79 g. (0.01 moles) of 3-hydroxy-3-methylglutaric acid monoamide, ammonium salt is dissolved in 50 ml of water and the solution is passed through a 100 ml column of Dowex 50 (H30 ) resin. The eluate is evaporated to dryness and the resulting residue dissolved in 100 ml of methanol containing 5 g. of hydrogen chloride. After 24 hours at room temperature the reaction mixture is evaporated to dryness under vacuum. The resulting residue is dissolved in 50 ml of water and the solution passed through a 50 ml column of Dowex 2 in the formate form. The column is eluted with 200 ml of water which is collected and evaporated under vacuum to afford 3-hydroxy-3-methylglutaric acid monoamide, methyl ester.

後処理

  1. customThe eluate is evaporated to dryness
  2. dissolutionthe resulting residue dissolved in 100 ml of methanol containing 5 g
  3. customAfter 24 hours at room temperature the reaction mixture is evaporated to dryness under vacuum
  4. dissolutionThe resulting residue is dissolved in 50 ml of water
  5. washThe column is eluted with 200 ml of water which
  6. customis collected
  7. customevaporated under vacuum

出典と根拠

ORDレコード
ord-a1cace6f994a4cb09ba0a9a7ff45839e
出典データセット
uspto-grants-1980_06
特許番号
US04208204

反応ノート

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