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Lithium Carbonate → Tert.-butyl 3-isopropyl-2-oxo-3-butenoate

HRID 1578920
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HRID 1578920 반응식
[Br-].[Li+].Cl[C:4]1([O:17][C:12]1([CH:14]([CH3:16])[CH3:15])[CH3:13])[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6].C(=O)([O-])[O-].[Li+].[Li+]>O>[CH:14]([C:12](=[CH2:13])[C:4](=[O:17])[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6])([CH3:16])[CH3:15]
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참가 물질

5

반응물 3

HCID 11125Lithium CarbonateHCID 82050Lithium BromideHCID 21443884Tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate

생성물 1

HCID 21405096Tert.-butyl 3-isopropyl-2-oxo-3-butenoate수율 85.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
5 °C

실험 절차

118 g of anhydrous lithium bromide were added under an inert atmosphere to a mixture of 117.5 g of tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate and 18.5 g of lithium carbonate in 1.15 liters of hexamethylphosphonotriamide cooled to 5°C and after the temperature was returned to room temperature, the mixture was stirred under a nitrogen atmosphere for 48 hours. 500 ml of distilled water were added thereto and the mixture was poured into an ampoule containing a mixture of water-petroleum ether (9-1). The mixture was decanted and the aqueous phase was extracted with petroleum ether. The combined ether phases were washed with water, dried over magnesium sulfate and the petroleum ether was evaporated under reduced pressure to obtain 84.6 g of tert.-butyl 3-isopropyl-2-oxo-3-butenoate.

후처리

  1. customwas returned to room temperature
  2. additionthe mixture was poured into an ampoule
  3. additioncontaining
  4. customThe mixture was decanted
  5. extractionthe aqueous phase was extracted with petroleum ether
  6. washThe combined ether phases were washed with water
  7. dry with materialdried over magnesium sulfate
  8. customthe petroleum ether was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-695813a9a28f462ab62abcce2f38987c
출처 데이터셋
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03940354

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