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

HRID 1361663

反应方程式

HRID 1361663 反应方程式
[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]

参与物

6

反应物 3

HCID 702乙醇HCID 1118四氧化硫HCID 27790153-硝基-4-三氟甲基苯甲酸

产物 1

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

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 8857乙酸乙酯溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-239bb387f3e949059ac6268ec44f034b
来源数据集
uspto-grants-2011_02
专利号
US07880000B2

关联笔记

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