Hydrochloric Acid → ethyl 4-(3,4-dichlorophenyl)-2,4-dioxobutanoate

HRID 539650

반응식

HRID 539650 반응식
CC([O-])(C)C.[K+].[CH3:7][C:8]([C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([Cl:17])[CH:11]=1)=[O:9].[CH2:18]([O:20][C:21](=[O:27])[C:22](OCC)=[O:23])[CH3:19].Cl>C1C=CC=CC=1>[Cl:17][C:12]1[CH:11]=[C:10]([C:8](=[O:9])[CH2:7][C:22](=[O:23])[C:21]([O:20][CH2:18][CH3:19])=[O:27])[CH:15]=[CH:14][C:13]=1[Cl:16]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 75841Ethanone, 1-(3,4-dichlorophenyl)-HCID 23665647Potassium tert-butoxide

생성물 1

HCID 10017017ethyl 4-(3,4-dichlorophenyl)-2,4-dioxobutanoate

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a solution of t-BuOK (0.05 mol, 5.6 g) in benzene (200 mL) was added dropwise a benzene (50 mL) solution of 3,4-dichloroacetophenone 5.1 (0.05 mol, 9.45 g) and diethyloxalate (0.055 mol, 8.1 g). The resultant mixture was stirred for 8 h at room temperature, then 10% aqueous HCl solution (100 mL) was added to the mixture. The organic layer was separated and washed with brine, dried over sodium sulfate and concentrated in vacuo. The crude product was purified by column chromatography using dichloromethane as eluent to yield the title compound. Yield: 7.5 g (52%).

후처리

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-1934ae3a8e0442dda759df426fd55823
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871761B2

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