Water → Ethyl 2-(4-nitrophenyl)propionate

HRID 261032

反応式

HRID 261032 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:6][CH:5]=1)([O-:3])=[O:2].[H-].[Na+].[CH3:18]I.O>CN(C)C=O.C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH:10]([CH3:18])[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:8][CH:9]=1)([O-:3])=[O:2]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 79517Ethyl 4-nitrophenylacetate

生成物 1

HCID 3016550Ethyl 2-(4-nitrophenyl)propionate

試薬・触媒・溶媒 1

HCID 21735183Dimethylformamide toluene溶媒

実験手順

To the solution of 52 g of ethyl 4-nitrophenylacetate in 350 ml dimethylformamide-toluene (1:1), 9.5 g of 50% sodium hydride in mineral oil are added portionwise while stirring and cooling. After 11/2 hours stirring at room temperature, 26 g methyl iodide are added dropwise and the mixture is stirred overnight at room temperature. The mixture is carefully combined with water, extracted with diethyl ether, the extract dried, filtered and evaporated. The residue is taken up in 100 ml ethanol, the solution seeded with a few crystals starting material and allowed to stand in the cold. The precipitate formed is filtered off and the filtrate evaporated, to yield the ethyl α-(4-nitrophenyl)-propionate.

後処理

  1. temperaturecooling
  2. stirringAfter 11/2 hours stirring at room temperature
  3. stirringthe mixture is stirred overnight at room temperature
  4. extractionextracted with diethyl ether
  5. customthe extract dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe precipitate formed
  9. filtrationis filtered off
  10. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-1a048898b4bd4afa81dd5b9c5bae27cf
出典データセット
uspto-grants-1979_08
特許番号
US04163788

関連ノート

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