Valproic Acid → Magnesium;bis(2-propylpentanoate);hydrate

HRID 1455718

反応式

HRID 1455718 の反応式
C(O)(=[O:9])C(CCC)CCC.[O-]CC.[Mg+2:14].[O-]CC.C(#N)C.[C:21]([O-:30])(=[O:29])[CH:22]([CH2:26][CH2:27][CH3:28])[CH2:23][CH2:24][CH3:25].[Mg+2].[C:32]([O-:41])(=[O:40])[CH:33]([CH2:37][CH2:38][CH3:39])[CH2:34][CH2:35][CH3:36]>C(O)C>[OH2:9].[C:21]([O-:30])(=[O:29])[CH:22]([CH2:26][CH2:27][CH3:28])[CH2:23][CH2:24][CH3:25].[Mg+2:14].[C:32]([O-:41])(=[O:40])[CH:33]([CH2:37][CH2:38][CH3:39])[CH2:34][CH2:35][CH3:36]

参加物

6

反応物 4

HCID 3121Valproic AcidHCID 6342AcetonitrileHCID 147515Magnesium ValproateHCID 164963Magnesium ethanolate

生成物 1

HCID 71439018Magnesium;bis(2-propylpentanoate);hydrate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of magnesium valproate in absolute ethanol was obtained in the following manner. To a magnetically stirred, clear, colorless solution of valproic acid (31.7 g; 0.22 mol; Sigma Aldrich Chemical Co.) in 200 mL of absolute ethanol was added 11.4 g (0.1 mol) of magnesium ethoxide solid; residual solid was rinsed in with 1 mL of absolute ethanol. Within 30 minutes, a clear, pale yellow solution was obtained; no increase in reaction temperature was observed. Acetonitrile (150 mL) was added to the ethanol solution in portions, and when the addition was complete a white precipitate formed. The reaction mixture was cold to the touch. The slurry was stirred for 15 minutes. The product, magnesium valproate hydrate, was isolated by filtration, washed with fresh acetonitrile, and dried to constant weight. The product, magnesium valproate hydrate, was obtained in 79.8% yield as a white solid, which exhibited an elemental composition identical to that calculated for magnesium valproate hydrate. The product did not melt at temperatures as high as 300° C. The product was not hygroscopic or deliquescent and was stable during storage under ambient conditions. The theoretical valproate content (weight %) of magnesium valproate hydrate is 88.6%; the valproate content found by HPLC analysis was 88.2%.

後処理

  1. washresidual solid was rinsed in with 1 mL of absolute ethanol
  2. customa clear, pale yellow solution was obtained
  3. temperatureno increase in reaction temperature
  4. additionthe addition
  5. customformed
  6. stirringThe slurry was stirred for 15 minutes

出典と根拠

ORDレコード
ord-b999b72626de48508ff58376fb6ebcb7
出典データセット
uspto-grants-2009_01
特許番号
US07482486B2

関連ノート

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