반응 #951027

반응 방정식

NaH

1-iodo-3-(2-phenylethoxy)propane

2-[4-(benzoxazol-2-yl)benzyloxy]ethylamine hydrochloride

→

N-[2-(4-(benzoxazol-2-yl)benzyloxy)ethyl]-3-(2-phenylethoxy)propanamine hydrochloride

용매

THF

반응 조건

후처리

1. 1
   온도The reaction mixture is heated
2. 2
   온도at reflux for 30 minutes
3. 3
   온도cooled
4. 4
   농축concentrated in vacuo
5. 5
   기타the residue column chromatographed with 10% MeOH/CH2Cl2The product
6. 6
   workup.DISSOLUTIONis dissolved in EtOH
7. 7
   농축concentrated to a solid
8. 8
   기타recrystallized from CH2Cl2 /petroleum ether

실험 절차

To a solution of 1-iodo-3-(2-phenylethoxy)propane (0.566 g; 1.95 mmol) in dry THF (9 ml) is added 2-[4-(benzoxazol-2-yl)benzyloxy]ethylamine hydrochloride (0.59 g; 1.9 mmol). NaH (78 mg; 1.9 mmol) is then added at room temperature. The reaction mixture is heated at reflux for 30 minutes, then cooled, concentrated in vacuo, and the residue column chromatographed with 10% MeOH/CH2Cl2The product is dissolved in EtOH acidified with HCl/EtOH concentrated to a solid and recrystallized from CH2Cl2 /petroleum ether to obtain N-[2-(4-(benzoxazol-2-yl)benzyloxy)ethyl]-3-(2-phenylethoxy)propanamine hydrochloride. (m.p. 134°-135° C.).

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