Hydrochloric Acid → 4-(2,4-Bis-benzyloxy-5-bromo-phenyl)-2,4-dioxo-butyric acid ethyl ester

HRID 646485노트

반응식

HRID 646485 반응식
[Na].[CH2:2]([O:9][C:10]1[CH:15]=[C:14]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:13]([Br:24])=[CH:12][C:11]=1[C:25](=[O:27])[CH3:26])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:28](OCC)(=[O:34])[C:29]([O:31][CH2:32][CH3:33])=[O:30].Cl>C(O)C>[CH2:32]([O:31][C:29](=[O:30])[C:28](=[O:34])[CH2:26][C:25]([C:11]1[CH:12]=[C:13]([Br:24])[C:14]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[CH:15][C:10]=1[O:9][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:27])[CH3:33]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 5360545SodiumHCID 247744411-(2,4-Bis-benzyloxy-5-bromo-phenyl)-ethanone

생성물 1

HCID 592648154-(2,4-Bis-benzyloxy-5-bromo-phenyl)-2,4-dioxo-butyric acid ethyl ester

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

9.75 g sodium (0.424 mol, 3 eq) were dissolved in 500 ml absolute ethanol (1.5 hours). 58 g of 1-(2,4-Bis-benzyloxy-5-bromo-phenyl)-ethanone (0.141 mol, 1 eq) and 30.98 g diethyl oxalate (0.212 mol, 1.5 eq) were added and the mixture was refluxed for 2 hours. After cooling down, the mixture was poured onto 220 ml of 2N aqueous HCl and the product was extracted into 700 ml dichloromethane. The solvent was removed under reduced pressure and the yellow residue was triturated with 150 ml diethyl ether.

후처리

  1. temperaturethe mixture was refluxed for 2 hours
  2. temperatureAfter cooling down
  3. extractionthe product was extracted into 700 ml dichloromethane
  4. customThe solvent was removed under reduced pressure
  5. customthe yellow residue was triturated with 150 ml diethyl ether

출처 및 근거

ORD 기록
ord-a7097c048399496c9d659cdbe0b61044
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07705027B2

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