Ethanol → Ethyl 3-nitro-4-(trifluoromethyl)benzoate

HRID 446312

반응식

HRID 446312 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[C:13]([F:16])([F:15])[F:14])[C:7]([OH:9])=[O:8])([O-:3])=[O:2].S(=O)(=O)(O)O.[CH2:22](O)[CH3:23]>C(OCC)(=O)C.O>[N+:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[C:13]([F:14])([F:15])[F:16])[C:7]([O:9][CH2:22][CH3:23])=[O:8])([O-:3])=[O:2]

참가 물질

6

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 27790153-Nitro-4-(trifluoromethyl)benzoic acid

생성물 1

HCID 19783148Ethyl 3-nitro-4-(trifluoromethyl)benzoate

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

3-Nitro-4-(trifluoromethyl)benzoic acid (10 g, 43 mmol) was taken up in 100 ml of ethanol and sulfuric acid (11 ml) was added to the mixture. The reaction was heated to reflux for 12 hours. The volatiles were removed in vacuo. The residue obtained was diluted with ethyl acetate and water. The layers were separated and the organic layer was washed with an aqueous solution of saturated sodium bicarbonate, water and brine. The organic layer was then dried with sodium sulfate and the volatiles removed in vacuo to give ethyl 3-nitro-4-(trifluoromethyl)benzoate a clear yellow oil.

후처리

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 12 hours
  3. customThe volatiles were removed in vacuo
  4. customThe residue obtained
  5. customThe layers were separated
  6. washthe organic layer was washed with an aqueous solution of saturated sodium bicarbonate, water and brine
  7. dry with materialThe organic layer was then dried with sodium sulfate
  8. customthe volatiles removed in vacuo

출처 및 근거

ORD 기록
ord-b05d94699b224a798d9286fa064a6e48
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476434B2

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