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

HRID 620808ノート

反応式

HRID 620808 の反応式
[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]

参加物

7

反応物 4

HCID 962WaterHCID 78341,2-Epoxybutane2 回HCID 8868Ethyl Acetoacetate2 回HCID 14798Sodium Hydroxide

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d292a9983997441cbb60be08acd78418
出典データセット
uspto-grants-1989_04
特許番号
US04822813

反応ノート

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