Water → Ethyl 2-formylbiphenyl-4-carboxylate

HRID 2264315ノート

反応式

HRID 2264315 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 23112255Ethyl 2-formylbiphenyl-4-carboxylate収率 66.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-39d4fcae014745ec80f8fc90aaa7d548
出典データセット
uspto-grants-2010_12
特許番号
US07855198B2

反応ノート

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