肼(无水) → 4-(3-chlorophenyl)butanoic Acid

HRID 2129

反应方程式

HRID 2129 反应方程式
[OH-].[K+].[Cl:3][C:4]1[CH:5]=[C:6]([CH:14]=[CH:15][CH:16]=1)[C:7]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])=O.NN>C(O)COCCO>[Cl:3][C:4]1[CH:5]=[C:6]([CH2:7][CH2:9][CH2:10][C:11]([OH:13])=[O:12])[CH:14]=[CH:15][CH:16]=1

参与物

5

反应物 3

HCID 9321肼(无水)HCID 14797氢氧化钾HCID 27578284-(3-氯苯基)-4-氧代丁酸

产物 1

HCID 113215684-(3-chlorophenyl)butanoic Acid收率 90.8%

试剂、催化剂与溶剂 1

HCID 8117二乙二醇溶剂

实验过程

To a 300 ml round-bottomed flask equipped with magnetic stirrer and reflux condenser was charged 23.7 g of 87% potassium hydroxide and 150 ml of diethyleneglycol, With stirring, 23 g of 3-(3-chlorobenzoyl)propionic acid was added followed by 24 g of 85% hydrazine. The mixture was heated to reflux for 2 hours when 50 ml of solvent was azeotroped off into a Dean-Stark trap. The reaction was refluxed for an additional 2 hours, cooled, and poured into 500 g of ice with 50 ml of con. hydrochloric acid. A white precipitate was formed which was extracted into 400 ml of ethyl ether, and washed with 100 ml of water and 100 ml of saturated sodium chloride solution. The ether extract was dried over anhydrous magnesium sulfate, filtered, and stripped to yield 19.5 g of product as a white solid.

后处理

  1. customTo a 300 ml round-bottomed flask equipped with magnetic stirrer
  2. temperaturereflux condenser
  3. temperatureThe mixture was heated
  4. customwas azeotroped off into a Dean-Stark trap
  5. temperatureThe reaction was refluxed for an additional 2 hours
  6. temperaturecooled
  7. additionpoured into 500 g of ice with 50 ml of con
  8. customA white precipitate was formed which
  9. extractionwas extracted into 400 ml of ethyl ether
  10. washwashed with 100 ml of water and 100 ml of saturated sodium chloride solution
  11. extractionThe ether extract
  12. dry with materialwas dried over anhydrous magnesium sulfate
  13. filtrationfiltered

来源与证据

ORD记录
ord-9f7ecc08ca4a459c8bd54d42b7e2aa72
来源数据集
uspto-grants-1998_03
专利号
US05728698

关联笔记

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