Water → Ethyl 2-(4-nitrophenyl)propionate

HRID 444538노트

반응식

HRID 444538 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 3016550Ethyl 2-(4-nitrophenyl)propionate

시약·촉매·용매 1

HCID 21735183Dimethylformamide toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ac512fdcae7c47bcb4798a1d0a2ccd28
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04264619

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