Potassium Carbonate → HCID 69439208、化合物

HRID 1350072ノート

反応式

HRID 1350072 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][C:10]#[N:11])[CH:6]=[CH:7][CH:8]=1.[H-].[Na+].[C:14](=O)([O:17]C)[O:15][CH3:16].C(=O)([O-])[O-].[K+].[K+]>C1COCC1.O>[C:10]([CH:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1)[C:14]([O:15][CH3:16])=[O:17])#[N:11]

参加物

7

反応物 4

HCID 11430Potassium Carbonate2 回HCID 12021Dimethyl CarbonateHCID 24758Sodium hydrideHCID 88310(3-Methoxyphenyl)acetonitrile

生成物 1

HCID 69439208HCID 69439208、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Twenty five grams of (3-methoxyphenyl)acetonitrile are dissolved in 200 ml of anhydrous THF in an Erlermeyer ground-necked flask. 60% sodium hydride (8.88 g; 0.37 mol) is added to the solution and the reaction mixture is heated at reflux for 30 minutes with stirring. Dimethyl carbonate (58 ml; 0.6814 mol) is then added dropwise in the course of half an hour and the reaction mixture is subsequently heated at reflux for 2 hours with stirring. The reaction mixture is poured into cold and slightly acidic water. The aqueous phase is extracted with ether, and then the ethereal phase is washed with water before being evaporated. A solution of potassium carbonate (47.15 g; 0.34 mol ) is added to the oil obtained above. After stirring, the mixture is washed with ether. The ethereal phase obtained is rewashed with a solution of potassium carbonate (12.02 g; 0.08 mol). The two aqueous phases are combined, immediately acidified, and extracted with ether. The organic phase so obtained is washed with a 10% sodium hydrogen carbonate solution, dried over magnesium sulphate and evaporated under reduced pressure to yield the title product in the form of an orangey yellow oil.

後処理

  1. temperaturethe reaction mixture is heated
  2. temperatureat reflux for 30 minutes
  3. temperaturethe reaction mixture is subsequently heated
  4. temperatureat reflux for 2 hours
  5. stirringwith stirring
  6. extractionThe aqueous phase is extracted with ether
  7. washthe ethereal phase is washed with water
  8. custombefore being evaporated
  9. customobtained above
  10. stirringAfter stirring
  11. washthe mixture is washed with ether
  12. customThe ethereal phase obtained
  13. extractionextracted with ether
  14. customThe organic phase so obtained
  15. washis washed with a 10% sodium hydrogen carbonate solution
  16. dry with materialdried over magnesium sulphate
  17. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-41186302b0914158a82bdadf90f8010b
出典データセット
uspto-grants-2007_05
特許番号
US07214689B2

反応ノート

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