Pyridine → N-allyl-allylsuccinimide

HRID 1722414

反応式

HRID 1722414 の反応式
[CH2:1]([CH:4]1[CH2:9][C:8](=[O:10])[O:7][C:5]1=O)[CH:2]=[CH2:3].[Na].[N:12]1C=C[CH:15]=[CH:14][CH:13]=1>C(OCC)C>[CH2:13]([N:12]1[C:8](=[O:10])[CH2:9][CH:4]([CH2:1][CH:2]=[CH2:3])[C:5]1=[O:7])[CH:14]=[CH2:15]

参加物

5

反応物 3

HCID 1049PyridineHCID 1110093-Allyl(dihydro)furan-2,5-dioneHCID 5360545Sodium

生成物 1

HCID 20028798N-allyl-allylsuccinimide収率 89.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

About 140 g (1 mol) of allylsuccinic anhydride and 250 ml of diethyl ether which has been dried over metallic sodium are placed under nitrogen in a round-bottomed flask equipped with a stirrer, dropping funnel and reflux condenser, and then mixed with 75 g (0.95 mol) of pyridine. About 57 g of allylamine in 100 ml of diethyl ether which has been dried over metallic sodium are then added dropwise to the flask with stirring over a period of 2 hours. When the addition is complete, the mixture is refluxed for an additional 1 hour. The resultant mixture is washed in a separating funnel with 5 percent aqueous hydrochloric acid until the pH of the aqueous phase is 6.5. The organic phase is dried over magnesium sulfate. After filtering off the drying agent, the solvent is removed at 15 hPa (abs.). About 153 g of N-allyl-allylsuccinimide, which boils at 130° C. at 0.5 hPa, are obtained from the residue by distillation.

後処理

  1. customare placed under nitrogen in a round-bottomed flask
  2. customequipped with a stirrer
  3. temperaturereflux condenser
  4. dry with materialAbout 57 g of allylamine in 100 ml of diethyl ether which has been dried over metallic sodium
  5. additionare then added dropwise to the flask
  6. additionWhen the addition
  7. temperaturethe mixture is refluxed for an additional 1 hour
  8. washThe resultant mixture is washed in a separating funnel with 5 percent aqueous hydrochloric acid until the pH of the aqueous phase
  9. dry with materialThe organic phase is dried over magnesium sulfate
  10. filtrationAfter filtering off the drying agent
  11. customthe solvent is removed at 15 hPa (abs.)

出典と根拠

ORDレコード
ord-c1f7fbf6679b43378244b70c39153c3a
出典データセット
uspto-grants-1989_08
特許番号
US04855378

関連ノート

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