Hydrochloric Acid → Ethyl 4-(furan-2-yl)-2,4-dioxobutanoate

HRID 33247

반응식

HRID 33247 반응식
C(O[C:4](=[O:10])[C:5]([O:7][CH2:8][CH3:9])=[O:6])C.CC([O-])(C)C.[K+].[O:17]1[CH:21]=[CH:20][CH:19]=[C:18]1[C:22](=[O:24])[CH3:23].Cl>C1COCC1.C(OCC)(=O)C.O>[CH2:8]([O:7][C:5](=[O:6])[C:4](=[O:10])[CH2:23][C:22]([C:18]1[O:17][CH:21]=[CH:20][CH:19]=1)=[O:24])[CH3:9]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 145052-AcetylfuranHCID 23665647Potassium tert-butoxide

생성물 1

HCID 3006753Ethyl 4-(furan-2-yl)-2,4-dioxobutanoate

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 16 g oxalic acid diethyl ester in 350 ml THF, 10.1 g KOt-Bu were added at 0° C. Then 10 g 1-furan-2-yl-ethanone in 50 ml THF were added dropwise. After 1 h the reaction mixture was diluted with 300 ml ethyl acetate and 200 mnl water. This solution was acidified with diluted hydrochloric acid to pH 5. The organic layer was separated, washed with 150 ml water, dried over MgSO4, filtered and concentrated under reduced pressure to yield a white solid.

후처리

  1. customThe organic layer was separated
  2. washwashed with 150 ml water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customto yield a white solid

출처 및 근거

ORD 기록
ord-4c8badb3b96b4d3aa4e6dc9d0f230fe0
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429581B2

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