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Dimethylformamide dimethyl acetal → HCID 54017096、化合物

HRID 1290823
ノート
印刷プレビュー

反応式

HRID 1290823 の反応式
[C:1]([O:9][CH:10]([CH3:14])[C:11](=[O:13])[CH3:12])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CO[CH:17](OC)[N:18]([CH3:20])[CH3:19]>>[C:1]([O:9][CH:10]([CH3:14])[C:11](=[O:13])[CH:12]=[CH:17][N:18]([CH3:20])[CH3:19])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 2319833-Oxobutan-2-yl benzoate

生成物 1

HCID 54017096HCID 54017096、化合物

実験手順

A mixture of 3-benzoyloxybutan-2-one (15.5 g) and dimethylformamide dimethylacetal (14.4 g) was heated on a steam bath for 2 hours 30 minutes. The solvent was removed from the mixture under reduced pressure. Petroleum ether (b.p. 60°-80° C.) was added to the residue, with shaking and the ether layer separated from an insoluble red oil. Further petroleum ether was added to the oil with shaking and excess ether was removed under reduced pressure to give a red-brown oil which partially crystallised on standing overnight. Petroleum ether was added and the solid was collected by filtration and washed with petroleum ether to give a yellow crystalline solid of 4-benzoyloxy-1-dimethylamino-1-penten-3-one. Yield 5.6 g. The solid was used directly without further purification in the next step.

後処理

  1. temperaturewas heated on a steam bath for 2 hours 30 minutes
  2. custom
The solvent was removed from the mixture under reduced pressure
  • additionPetroleum ether (b.p. 60°-80° C.) was added to the residue
  • customthe ether layer separated from an insoluble red oil
  • additionFurther petroleum ether was added to the oil
  • stirringwith shaking
  • customexcess ether was removed under reduced pressure
  • customto give a red-brown oil which
  • custompartially crystallised
  • additionPetroleum ether was added
  • filtrationthe solid was collected by filtration
  • washwashed with petroleum ether
  • 出典と根拠

    ORDレコード
    ord-d5e221e9437649fca574fea1b2a00e2c
    出典データセット
    uspto-grants-1998_05
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US05753665

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