Water → Ethyl 2-formylbiphenyl-4-carboxylate

HRID 731929노트

반응식

HRID 731929 반응식
Br[CH2:2][C:3]1[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[CH:5][C:4]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C[N+]1([O-])CC[O:24]CC1.O>C(#N)C>[CH:2]([C:3]1[CH:8]=[C:7]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:6]=[CH:5][C:4]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[O:24]

참가 물질

5

반응물 3

HCID 962WaterHCID 82029Methyl morpholine oxideHCID 23112214Ethyl 2-(bromomethyl)biphenyl-4-carboxylate

생성물 1

HCID 23112255Ethyl 2-formylbiphenyl-4-carboxylate수율 66.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

In 100 ml of acetonitrile was dissolved 9.3 g of ethyl 2-(bromomethyl)biphenyl-4-carboxylate, and 7.0 g of N-methylmorpholine-N-oxide was added thereto at room temperature, followed by 4 hours of stirring. Water was added to the reaction solution, which was then extracted with ethyl acetate. The resulting organic layer was dried over anhydrous magnesium sulfate. After the solvent was removed by evaporation, the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate) to obtain 4.94 g of ethyl 2-formylbiphenyl-4-carboxylate as a white solid.

후처리

  1. additionwas added
  2. extractionwas then extracted with ethyl acetate
  3. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  4. customAfter the solvent was removed by evaporation
  5. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate)

출처 및 근거

ORD 기록
ord-98154ab59f1f4f2585d1fb8f3e60d177
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585878B2

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