Ethyl Acetoacetate → Ethyl 2-acetyl-3-methyl-4-oxopentanoate

HRID 127757

반응식

HRID 127757 반응식
[Na].[C:2]([O:8][CH2:9][CH3:10])(=[O:7])[CH2:3][C:4]([CH3:6])=[O:5].[O-]CC.[Na+].Br[CH:16]([CH3:20])[C:17](=[O:19])[CH3:18]>C(O)C>[CH2:9]([O:8][C:2]([CH:3]([CH:16]([CH3:20])[C:17](=[O:19])[CH3:18])[C:4](=[O:5])[CH3:6])=[O:7])[CH3:10]

참가 물질

6

반응물 4

HCID 8868Ethyl AcetoacetateHCID 131422-Butanone, 3-bromo-HCID 2723922Sodium ethoxideHCID 5360545Sodium

생성물 1

HCID 14689360Ethyl 2-acetyl-3-methyl-4-oxopentanoate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

7.3 G., 0.317 mol of sodium was dissolved in 125 ml. of absolute ethanol 87.0 G. (0.669 mol) of ethyl acetoacetate were added to the resulting solution of sodium ethoxide in the cold. The reaction mixture was heated to reflux and 48.6 g. (0.322 mol) of freshly distilled 3-bromo-2-butanone were added dropwise with stirring over a period of 30 min. Refluxing was continued until the mixture tested neutral to pH paper (~1.5 hrs.). The precipitated sodium bromide was filtered off the cold solution and most of the ethanol was removed on an evaporator. The mixture was filtered again and distilled. The 3-ethoxycarbonyl-4-methyl-hexane-2,4-dione fraction which boiled at 131°-137° C./18 mm. was collected.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. temperatureRefluxing
  4. customtested neutral to pH paper (~1.5 hrs.)
  5. filtrationThe precipitated sodium bromide was filtered off the cold solution
  6. custommost of the ethanol was removed on an evaporator
  7. filtrationThe mixture was filtered again
  8. distillationdistilled
  9. customwas collected

출처 및 근거

ORD 기록
ord-e4e4ce6b926d4505b8a6a5bfaade3f85
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256878

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