1,3-Butanedione, 1-(2-furanyl)- → 3-Amino-1-(2-furanyl)-2-buten-1-one

HRID 1285365

반응식

HRID 1285365 반응식
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6](=[O:11])[CH2:7][C:8](=O)[CH3:9].C([O-])(=O)C.[NH4+:16]>C1(C)C=CC=CC=1>[NH2:16][C:8]([CH3:9])=[CH:7][C:6]([C:2]1[O:1][CH:5]=[CH:4][CH:3]=1)=[O:11]

참가 물질

4

반응물 2

HCID 121681,3-Butanedione, 1-(2-furanyl)-HCID 517165Ammonium Acetate

생성물 1

HCID 704481453-Amino-1-(2-furanyl)-2-buten-1-one수율 48.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

The intermediate 3-amino-1-(2-furanyl)-2-buten-1-one was prepared as follows: A mixture containing 165 g of 1-(2-furanyl)-1,3-butanedione, 700 ml of toluene and 200 g of ammonium acetate was azeotroped for six hours, cooled and concentrated to dryness in vacuo. The residue was dissolved in isopropyl alcohol, the solution treated with decolorizing charcoal and filtered, and the filtrate concentrated to remove the solvent. The remaining residue was recrystallized from ether-ethanol and dried at room temperature to yield 80.2 g of 3-amino-1-(2-furanyl)-2-buten-1-one, m.p. 128°-130° C. Another 33.4 g of the product, m.p. 128°-130° C. was collected by concentrating the mother liquor and extracting the product with ether.

후처리

  1. customThe intermediate 3-amino-1-(2-furanyl)-2-buten-1-one was prepared
  2. customwas azeotroped for six hours
  3. temperaturecooled
  4. concentrationconcentrated to dryness in vacuo
  5. dissolutionThe residue was dissolved in isopropyl alcohol
  6. additionthe solution treated with decolorizing charcoal
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated
  9. customto remove the solvent
  10. customThe remaining residue was recrystallized from ether-ethanol
  11. customdried at room temperature

출처 및 근거

ORD 기록
ord-1209be109e7249fea50eda207f6951dc
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04567186

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