Hydrochloric Acid → Ethyl 4,4-diethoxy-3-oxobutanoate

HRID 515878노트

반응식

HRID 515878 반응식
[CH2:1]([O:3][CH:4]([O:10][CH2:11][CH3:12])[C:5]([O:7]CC)=O)[CH3:2].[Na].CO.Cl.[C:17]([O:20][CH2:21][CH3:22])(=[O:19])[CH3:18]>O>[CH2:11]([O:10][CH:4]([O:3][CH2:1][CH3:2])[C:5](=[O:7])[CH2:18][C:17]([O:20][CH2:21][CH3:22])=[O:19])[CH3:12]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 887MethanolHCID 8857Ethyl AcetateHCID 80169Ethyl diethoxyacetateHCID 5360545Sodium

생성물 1

HCID 11138577Ethyl 4,4-diethoxy-3-oxobutanoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 40 g of ethyl diethoxyacetate (227 mmol) in 67 mL of ethyl acetate there are added under argon, in portions, 6 g of sodium (261 mmol). The reaction mixture is then stirred at ambient temperature for 48 hours. There are added 10 mL of methanol, and then the mixture is hydrolysed with 65 mL of water. The pH of the reaction mixture is adjusted to pH 6 by adding 1N aqueous HCl solution. The mixture is separated and then extracted with ethyl acetate. The organic phases are combined, washed with brine, dried over MgSO4, filtered and concentrated to dryness. The title product is obtained in the form of an oil which is used in the next Step without being otherwise purified.

후처리

  1. customThe mixture is separated
  2. extractionextracted with ethyl acetate
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-d9f46fe1de924c79b33b08ca572d0fd7
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108983B2

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