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Hydrochloric Acid → pentane-2,3,4-trione 4-(O-methyl oxime)-2-oxime

HRID 1636957
ノート
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反応式

HRID 1636957 の反応式
[N:1](OCCCC)=[O:2].C[O-].[Na+].[CH3:11][O:12][N:13]=[C:14]([C:16](=[O:19])[CH2:17][CH3:18])[CH3:15].Cl>CO>[CH3:11][O:12][N:13]=[C:14]([CH3:15])[C:16](=[O:19])[C:17](=[N:1][OH:2])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10996Butyl nitriteHCID 10942334Sodium MethoxideHCID 541960112,3-Pentanedione, 2-(O-methyloxime)

生成物 1

HCID 53804423pentane-2,3,4-trione 4-(O-methyl oxime)-2-oxime

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

10.3 g (0.1 mol) of n-butyl nitrite and then 54 g of a 30% strength solution of sodium methylate in methanol are carefully added dropwise at 10° C. to a solution of 12.9 g (0.1 mol) of pentane-2,3-dione 2-(O-methyl oxime) in 120 ml of methanol. The mixture is allowed to come to room temperature and is stirred for 12 hours at this temperature. The mixture is worked up by adding dilute hydrochloric acid to a pH of 7 and subsequent evaporation in vacuo. The residue is taken up in 100 ml of water and extracted twice using in each case 100 ml of diethyl ether. The organic phase is dried over sodium sulfate and evaporated in vacuo. This gives 7.7 g (49%) of an oil.

後処理

  1. customto come to room temperature
  2. customto a pH of 7 and subsequent evaporation in vacuo
  3. extractionextracted twice
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-df02c1ebe0e344c59a8f14993dc8e8e5
出典データセット
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06037378

反応ノート

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