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DL-norvaline → HCID 178440053、化合物

HRID 1075283
ノート
印刷プレビュー

反応式

HRID 1075283 の反応式
[N:1](=[C:3]([C:7](=[O:9])[CH3:8])[C:4](=O)[CH3:5])O.[NH2:10][CH:11](C(O)=O)[CH2:12][CH2:13][CH3:14]>C(O)CCC>[C:7]([C:3]1[NH:1][C:11]([CH2:12][CH2:13][CH3:14])=[N:10][C:4]=1[CH3:5])(=[O:9])[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 824DL-norvalineHCID 178468373HCID 178468373、化合物

生成物 1

HCID 178440053HCID 178440053、化合物収率 55.7%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To 40 g (0.309 moles) of 3-oximino-2,4-pentanedione dissolved in 200 ml of n-butanol was added 39.92 g (0.341 moles) of d,l-norvaline. The resulting mixture was brought to reflux, while stirring rapidly under nitrogen with an oil bath. After 19.3 h the reaction mixture was cooled, and then suction filtered. The residue was washed with ethyl acetate (100 ml) and the combined filtrates concentrated in vacuo. The resulting oil was dissolved in ethyl acetate (200 ml) and extracted with three 50 ml portions of 5% aqueous sodium hydroxide solution. Removal of the solvent in vacuo gave 0.15 moles (55.7% yield based on recovered d,l-norvaline) of 5-acetyl-4-methyl-2-propylimidazole.

後処理

  1. temperatureto reflux
  2. temperatureAfter 19.3 h the reaction mixture was cooled
  3. filtrationsuction filtered
  4. washThe residue was washed with ethyl acetate (100 ml)
  5. concentrationthe combined filtrates concentrated in vacuo
  6. dissolutionThe resulting oil was dissolved in ethyl acetate (200 ml)
  7. extractionextracted with three 50 ml portions of 5% aqueous sodium hydroxide solution
  8. customRemoval of the solvent in vacuo

出典と根拠

ORDレコード
ord-1bae31e2f000464f88f0fc0d04c6405d
出典データセット
uspto-grants-1983_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04395547

反応ノート

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