Water → 3-Acetyl-5-Ethyldihydro-2(3H)-Furanone

HRID 620808노트

반응식

HRID 620808 반응식
[CH2:1]([O:3][C:4](=[O:9])[CH2:5][C:6]([CH3:8])=[O:7])[CH3:2].O1[CH:12](CC)[CH2:11]1.[OH-].[Na+].O>C(O)(=O)C.C(O)C>[C:6]([CH:5]1[CH2:2][CH:1]([CH2:11][CH3:12])[O:3][C:4]1=[O:9])(=[O:7])[CH3:8]

참가 물질

7

반응물 4

HCID 962WaterHCID 78341,2-Epoxybutane2회HCID 8868Ethyl Acetoacetate2회HCID 14798Sodium Hydroxide

생성물 1

HCID 110518973-Acetyl-5-Ethyldihydro-2(3H)-Furanone수율 45%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 702Ethanol용매

실험 절차

2-acetyl-4-ethyl butyrolactone was prepared from ethylacetoacetate and 1,2-epoxybutane according to the method described in Johnson U.S. Pat. No. 2,443,827. A mixture of 40 g sodium hydroxide (1.0 mole), 270 ml water and 90 ml ethanol was cooled to 0°, stirred, and 130 g ethylacetoacetate (1.0 mole) and 72 g 1,2-epoxybutane (1.0 mole) added. Stirring was continued at 0°, and the mixture was thereafter left at 4° C. for 48 hours. The reaction mixture was neutralized with 80 ml acetic acid, extracted with toluene, washed with water, sodium bicarbonate and finally with water. The mixture was then dried (magnesium sulfate), filtered and the solvent removed, leaving a product, bp 86°-96°-/0.1 mm, in 45% yield.

후처리

  1. temperaturewas cooled to 0°
  2. stirringStirring
  3. customwas continued at 0°
  4. extractionextracted with toluene
  5. washwashed with water, sodium bicarbonate and finally with water
  6. dry with materialThe mixture was then dried (magnesium sulfate)
  7. filtrationfiltered
  8. customthe solvent removed
  9. customleaving a product, bp 86°-96°-/0.1 mm

출처 및 근거

ORD 기록
ord-d292a9983997441cbb60be08acd78418
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04822813

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