反应 #2006413

ord-0c1e62225c734ab4aad5681e0a5899dd

反应方程式

O=C([O-])O.[Na+]
NaHCO3
O=C([O-])[O-].[Na+].[Na+]
Na2CO3
Nc1ccc(CCCC(=O)O)cc1
4-(4-aminophenyl)-butyric acid
Cl
HCl
COC(=O)CCCc1ccc(N)cc1
40
收率 91.0%
COC(=O)CCCc1ccc(N)cc1
Methyl-4-(4-aminophenyl)-butanoate
收率 91.0%

溶剂

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was evaporated under reduced pressure
  2. 2
    萃取the aqueous phase was extracted several times with CH2Cl2
  3. 3
    其他The crude material was purified by flash chromatography

实验过程

To a solution of 4-(4-aminophenyl)-butyric acid (5 g, 27.90 mmol) in MeOH (100 mL) at room temperature was added HCl conc. (37% 15 mL). The resulting mixture was stirred overnight at 50° C. then treated with a saturated aqueous solution NaHCO3 and Na2CO3 solid until pH 9. The solvent was evaporated under reduced pressure then the aqueous phase was extracted several times with CH2Cl2. The crude material was purified by flash chromatography using CH2Cl2/MeOH as solvent mixture yielding 40 (4.93 g, 91%) as orange solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE043343E1uspto-grants-2012_05