γ-氨基丁酸 → 4-((苯磺酰基)氨基)丁酸

HRID 1921663笔记

反应方程式

HRID 1921663 反应方程式
[NH2:1][CH2:2][CH2:3][CH2:4][C:5]([OH:7])=[O:6].[C:8]1([S:14](Cl)(=[O:16])=[O:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>[OH-].[Na+]>[C:8]1([S:14]([NH:1][CH2:2][CH2:3][CH2:4][C:5]([OH:7])=[O:6])(=[O:16])=[O:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参与物

4

反应物 2

HCID 119γ-氨基丁酸HCID 7369苯磺酰氯

产物 1

HCID 3627414-((苯磺酰基)氨基)丁酸

试剂、催化剂与溶剂 1

HCID 14798氢氧化钠溶剂2 次

实验过程

7 G of gamma-aminobutyric acid was dissolved in 120 mL of 1N sodium hydroxide solution, and 15 g of benzenesulfonyl chloride was dropwise added thereto under ice-cooling. 2N sodium hydroxide solution was added to the mixture to adjust the pH to 9.2 and stirred for 4 hours. The stirred mixture was washed with 50 mL of ethyl acetate, and hydrochloric acid was added thereto to adjust the pH to 2 or less. After extracting with 500 mL of ethyl acetate, this was dried with magnesium sulfate and filtered. After a concentration under reduced pressure, the obtained residue was recrystallized with ethanol solution to give 13 g of the desired product.

后处理

  1. temperatureunder ice-cooling
  2. washThe stirred mixture was washed with 50 mL of ethyl acetate, and hydrochloric acid
  3. additionwas added
  4. extractionAfter extracting with 500 mL of ethyl acetate
  5. dry with materialthis was dried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationAfter a concentration under reduced pressure
  8. customthe obtained residue was recrystallized with ethanol solution

来源与证据

ORD记录
ord-159bc24f5f5b4301b1ce38d4e2935c8c
来源数据集
uspto-grants-2012_05
专利号
US08173705B2

反应笔记

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