(2-Methyl-2-propenyl)succinic Anhydride → 3-isobutyldihydrofuran-2,5-dione

HRID 443188

反応式

HRID 443188 の反応式
[CH2:1]([CH:5]1[C:10](=[O:11])[O:9][C:7](=[O:8])[CH2:6]1)[C:2](=[CH2:4])[CH3:3].[H][H]>C1(C)C=CC=CC=1.[Pd]>[CH2:1]([CH:5]1[CH2:6][C:7](=[O:8])[O:9][C:10]1=[O:11])[CH:2]([CH3:4])[CH3:3]

参加物

5

反応物 2

HCID 225375(2-Methyl-2-propenyl)succinic AnhydrideHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 104871113-isobutyldihydrofuran-2,5-dione収率 97.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1140Toluene溶媒

実験手順

β-Methallylsuccinic anhydride (539 g, 3.50 mole) was dissolved in toluene (800 mL) in a 1700 mL Parr stainless steel bottle fitted with a heating jacket. 10% Pd/C (3.60 g) was added and the bottle was connected to a Parr 2 L shaker fitted with two 4 L hydrogen tanks. After several evacuations and refilling with hydrogen, the shaker was started with the heater controlled for 60° C. The initial pressure was 60 lbs. When the pressure fell to 10 lbs, the tanks were repressurized to 60 lbs. After two hours, the controller was reset to 70° C. and the reaction was continued for another 12 hours. The heat was then turned off and after another 5 hours, the shaker was stopped. The reaction vessel was evacuated and the reaction mixture was filtered and concentrated. Distillation of the residue through the Vigreux column described above (P=9-10 mm Hg, T=180° C.) gave isobutylsuccinic anhydride (532.9 g, 97.6% yield).

後処理

  1. customfitted with a heating jacket
  2. customcontrolled for 60° C
  3. customwas reset to 70° C.
  4. waitthe reaction was continued for another 12 hours
  5. waitThe heat was then turned off and after another 5 hours
  6. customThe reaction vessel was evacuated
  7. filtrationthe reaction mixture was filtered
  8. concentrationconcentrated
  9. distillationDistillation of the residue through the Vigreux column
  10. customdescribed above (P=9-10 mm Hg, T=180° C.)

出典と根拠

ORDレコード
ord-01ec35a4b0004e90bd60299a863dcfa1
出典データセット
uspto-grants-1999_04
特許番号
US05892112

関連ノート

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