反応 #1003679

ord-c8e20f890da04c3e8d60e09bd7268c1d

溶媒

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE039850E1uspto-grants-2007_09