海萝胶 → 3-(4-乙基苯甲酰)丙酸

HRID 2886

反应方程式

HRID 2886 反应方程式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)[CH3:2].[Cl-].[Al+3].[Cl-].[Cl-].[C:13]1(=[O:19])[O:18][C:16](=[O:17])[CH2:15][CH2:14]1.Cl>>[O:19]=[C:13]([C:6]1[CH:7]=[CH:8][C:3]([CH2:1][CH3:2])=[CH:4][CH:5]=1)[CH2:14][CH2:15][C:16]([OH:18])=[O:17]

参与物

5

反应物 4

HCID 313海萝胶HCID 7500乙基苯HCID 7922丁二酸酐HCID 6451240三氯化铝

产物 1

HCID 3169833-(4-乙基苯甲酰)丙酸

实验过程

5 cm3 of ethylbenzene and 2.6 g of aluminum chloride are mixed with magnetic stirring in a 50-cm3 flask. The solution is cooled in an ice bath and 1 g of succinic anhydride is then added. The reaction mixture is stirred for 1 h 30 min at a temperature of 0° C. and then for 3 h at room temperature. It is poured into ice. The resulting mixture is acidified by adding 1N hydrochloric acid (pH 3-4). It is extracted with 3 volumes of ether. The organic phases are washed 3 times with 10% potassium carbonate solution. The aqueous phases are combined and acidified by adding concentrated hydrochloric acid. The precipitate obtained is drained and then recrystallized.

后处理

  1. temperatureThe solution is cooled in an ice bath
  2. stirringThe reaction mixture is stirred for 1 h 30 min at a temperature of 0° C.
  3. additionIt is poured into ice
  4. extractionIt is extracted with 3 volumes of ether
  5. washThe organic phases are washed 3 times with 10% potassium carbonate solution
  6. additionby adding concentrated hydrochloric acid
  7. customThe precipitate obtained
  8. customrecrystallized

来源与证据

ORD记录
ord-14978e6518ec43e492e5f892cd564bb7
来源数据集
uspto-grants-1998_03
专利号
US05731352

关联笔记

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