海萝胶 → 3-Chloro-4-cyclohexylcinnamic acid

HRID 26562

反应方程式

HRID 26562 反应方程式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)[CH:5]=O.C(O)(=O)[CH2:17][C:18]([OH:20])=[O:19].N1CCCCC1.Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)[CH:5]=[CH:17][C:18]([OH:20])=[O:19]

参与物

6

反应物 4

HCID 313海萝胶HCID 867丙二酸2 次HCID 8082六氢吡啶HCID 107277773-Chloro-4-cyclohexylbenzaldehyde

产物 1

HCID 542933553-Chloro-4-cyclohexylcinnamic acid

试剂、催化剂与溶剂 1

HCID 1049吡啶溶剂

实验过程

3-Chloro-4-cyclohexylbenzaldehyde (0.1 mole), malonic acid (0.2 moles), and dry pyridine (175 ml) are placed in a 1 l round-bottom flask. The malonic acid is dissolved by shaking on a steam bath and piperidine (0.5 ml) is added. The reaction is allowed to take place on the steam bath for 4 hours. After standing at room temperature overnight, the mixture is refluxed for 1 hour and cooled. The reaction mixture is poured into 250 ml of ice water and acidified with concentrated hydrochloric acid (80 ml) with stirring. The crystals of product are collected by filtration, washed with water (4× 150 ml) and air dried. Recrystallization from acetone-water gives 3-chloro-4-cyclohexylcinnamic acid.

后处理

  1. customfor 4 hours
  2. temperaturethe mixture is refluxed for 1 hour
  3. temperaturecooled
  4. stirringwith stirring
  5. filtrationThe crystals of product are collected by filtration
  6. washwashed with water (4× 150 ml) and air
  7. customdried
  8. customRecrystallization from acetone-water

来源与证据

ORD记录
ord-3d9256a617834f628b42d114deddc829
来源数据集
uspto-grants-1979_04
专利号
US04150148

关联笔记

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