丙二酸 → (E)-3-(4-甲氧基-3-硝基-苯基)丙烯酸

HRID 470610

反应方程式

HRID 470610 反应方程式
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12].C(O)(=O)[CH2:15][C:16]([OH:18])=[O:17].N1CCCCC1>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH:7]=[CH:15][C:16]([OH:18])=[O:17])=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12]

参与物

5

反应物 3

HCID 867丙二酸HCID 8082六氢吡啶HCID 7006083-硝基-4-甲氧基苯甲醛

产物 1

HCID 821746(E)-3-(4-甲氧基-3-硝基-苯基)丙烯酸

试剂、催化剂与溶剂 1

HCID 1049吡啶溶剂3 次

反应条件

温度
120 °C

实验过程

4-methoxy-3-nitro-benzaldehyde (compound of Example 5; 1.05 g, 5.79 mmol) and malonic acid (1.32 g, 1.27 mmol) were dissolved in pyridine (20 mL) under stirring and piperidine (1 mL) was added to the pyridine solution. The reaction mixture was heated at 75° C. to 80° C. for 3 h, after which the temperature was further increased to 120° C. and maintained at this temperature for 6 h. At the end of the reaction, pyridine was evaporated, followed by addition of aqueous HCl (1:1) to obtain pH ˜4. The solid obtained was filtered, washed with cold water and dried.

后处理

  1. temperatureThe reaction mixture was heated at 75° C. to 80° C. for 3 h
  2. temperaturemaintained at this temperature for 6 h
  3. customwas evaporated
  4. additionfollowed by addition of aqueous HCl (1:1)
  5. customto obtain pH ˜4
  6. customThe solid obtained
  7. filtrationwas filtered
  8. washwashed with cold water
  9. customdried

来源与证据

ORD记录
ord-c9716e3dc2f346b3bd78114fc4c8aab5
来源数据集
uspto-grants-2014_01
专利号
US08629277B2

关联笔记

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