Acetone → Magnesium Valproate

HRID 1455715

반응식

HRID 1455715 반응식
[O-]CC.[Mg+2:4].[O-]CC.[C:8]([OH:17])(=[O:16])[CH:9]([CH2:13][CH2:14][CH3:15])[CH2:10][CH2:11][CH3:12].CC(C)=O>C(O)C>[C:8]([O-:17])(=[O:16])[CH:9]([CH2:13][CH2:14][CH3:15])[CH2:10][CH2:11][CH3:12].[Mg+2:4].[C:8]([O-:17])(=[O:16])[CH:9]([CH2:13][CH2:14][CH3:15])[CH2:10][CH2:11][CH3:12]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 3121Valproic AcidHCID 164963Magnesium ethanolate2회

생성물 1

HCID 147515Magnesium Valproate수율 66%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

11.4 g (0.1 mol) of magnesium ethoxide solid was added to a magnetically stirred, clear, colorless solution of valproic acid (28.8 g; 0.2 mol; Sigma Aldrich Chemical Co.) in 25 mL of absolute ethanol. Residual solid was rinsed into the reaction with 5 mL of absolute ethanol to provide a total volume of 30 mL of absolute ethanol. Within 10 minutes, the slurry became very warm to the touch, and the color of the solution phase changed to pale yellow. Complete dissolution of the magnesium ethoxide solid in ethanol was never achieved, but within minutes the solid phase converted from a slurry of a yellow granular solid to a suspension of white solid that was so thick that stirring stopped. 100 mL of acetone was added, and the thick slurry was stirred for 10 minutes. The precipitate was isolated by filtration, washed with fresh acetone, and dried to constant weight. The product, magnesium valproate, was obtained in 66% yield. Elemental analysis (Table 1) indicated that the product was an inhomogeneous mixture of magnesium valproate and other magnesium salts. The theoretical valproate content (%) of magnesium valproate is 92.2%; the valproate content found by HPLC analysis was 78.4%.

후처리

  1. washResidual solid was rinsed into the reaction with 5 mL of absolute ethanol
  2. customto provide a total volume of 30 mL of absolute ethanol
  3. temperaturethe slurry became very warm to the touch
  4. additionwithin minutes the solid phase converted from a slurry of a yellow granular solid to a suspension of white solid
  5. stirringthat stirring
  6. stirringthe thick slurry was stirred for 10 minutes
  7. customThe precipitate was isolated by filtration
  8. washwashed with fresh acetone
  9. customdried to constant weight

출처 및 근거

ORD 기록
ord-203ca7b4894e4ee18cd5db346712ff5d
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07482486B2

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