Hydrochloric Acid → Diethyl 3-difluoromethoxy-2,4,5-trifluorobenzoylmalonate

HRID 1440095ノート

反応式

HRID 1440095 の反応式
C([O-])(=O)CC([O-])=O.C(C(CC)(O[Mg+2])C)C.[O-]CC.[Mg+2].[O-]CC.[C:23]([O:31][CH2:32][CH3:33])(=[O:30])[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26].[F:34][CH:35]([F:49])[O:36][C:37]1[C:38]([F:48])=[C:39]([CH:43]=[C:44]([F:47])[C:45]=1[F:46])[C:40](Cl)=[O:41].Cl>C(OCC)C>[F:49][CH:35]([F:34])[O:36][C:37]1[C:38]([F:48])=[C:39]([CH:43]=[C:44]([F:47])[C:45]=1[F:46])[C:40]([CH:24]([C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:23]([O:31][CH2:32][CH3:33])=[O:30])=[O:41]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7761Diethyl MalonateHCID 164963Magnesium ethanolateHCID 152829712,4,5-Trifluoro-3-difluoromethoxybenzoyl chloride

生成物 1

HCID 15023783Diethyl 3-difluoromethoxy-2,4,5-trifluorobenzoylmalonate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

実験手順

Meanwhile, a suspension of diethyl ethoxymagnesium malonate in diethyl ether was prepared from a mixture of 2.80 g (0.0238 moles) of magnesium ethoxide and 3.81 g (0.0238 moles) of diethyl malonate in 60 ml of anhydrous diethyl ether by heating under reflux for 1 hour, whilst stirring. A solution of the 3-difluoromethoxy-2,4,5-trifluorobenzoyl chloride prepared as described above in 50 ml of anhydrous diethyl ether was then added dropwise to the suspension, whilst stirring at room temperature, and the mixture was then stirred at room temperature for an additional 2 hours. 35 ml of 1N aqueous hydrochloric acid were added to the reaction mixture, and the mixture was vigorously stirred. The organic layer was then separated, washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by evaporation under reduced pressure to give 7.07 g of diethyl 3-difluoromethoxy-2,4,5-trifluorobenzoylmalonate [(XIV), R1 =--OCHF2, R3' =H, R17 =C2H5, X=X'=F] as a brown liquid.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 1 hour
  3. additionwas then added dropwise to the suspension
  4. stirringwhilst stirring at room temperature
  5. stirringthe mixture was then stirred at room temperature for an additional 2 hours
  6. stirringthe mixture was vigorously stirred
  7. customThe organic layer was then separated
  8. washwashed with water
  9. dry with materialdried over anhydrous sodium sulfate
  10. customThe solvent was then removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-85cc3b5cac4e444c9922bc0952c797f7
出典データセット
uspto-grants-1996_03
特許番号
US05496951

反応ノート

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