反応 #322907

反応方程式

1,4-diaminobutane

2-{2-[(2,6-dichlorophenyl)-amino]-phenyl}-acetic acid p-nitrophenyl ester

→

2-{2-[(2,6-dichlorophenyl)-amino]-phenyl}-acetic acid 4-aminobutylamide hydrochloride

溶媒

methylene chloride methanol

反応条件

後処理

1. 1
   濃縮The reaction solution is then concentrated by evaporation in vacuo
2. 2
   抽出the whole is extracted
3. 3
   抽出The aqueous phase is extracted three times with diethyl ether
4. 4
   その他to remove nitrophenol
5. 5
   抽出saturated with NaCl and extracted with tetrahydrofuran
6. 6
   乾燥The organic phase is dried with Na2SO4
7. 7
   濃縮concentrated by evaporation
8. 8
   その他The residue is triturated with diethyl ether
9. 9
   その他yields a crystalline powder which
10. 10
    その他is recrystallised from ethyl acetate

実験手順

1,4-diaminobutane and 2-{2-[(2,6-dichlorophenyl)-amino]-phenyl}-acetic acid p-nitrophenyl ester are allowed to react for 8 hours at room temperature in methylene chloride/methanol (1:1). The reaction solution is then concentrated by evaporation in vacuo, the residue is taken up in tetrahydrofuran and the whole is extracted by shaking with 2N hydrochloric acid. The aqueous phase is extracted three times with diethyl ether to remove nitrophenol and is then saturated with NaCl and extracted with tetrahydrofuran. The organic phase is dried with Na2SO4 and concentrated by evaporation. The residue is triturated with diethyl ether and yields a crystalline powder which is recrystallised from ethyl acetate. 2-{2-[(2,6-dichlorophenyl)-amino]-phenyl}-acetic acid 4-aminobutylamide hydrochloride is obtained in the form of its ethyl acetate solvate; m.p. 137°-140°; Rf =0.177 (CHCl3 :methanol:concentrated aqueous ammonia solution=10:10:0.1).

出典