반응 #163379

반응 방정식

3-chloropivaloyl chloride

2-[4-(4-ethoxy-phenylethynyl)-phenyl]-1-methyl-ethylamine

K2CO3

→

1-{2-[4-(4-Ethoxy-phenylethynyl)-phenyl]-1-methyl-ethyl}-3,3-dimethyl-azetidin-2-one

용매

ACN

반응 조건

후처리

1. 1
   온도at reflux for 6 h
2. 2
   기타The solvent is removed in vacuo
3. 3
   세척washed with water (1×), sat. aq. NaHCO3 solution (2×) and again with water
4. 4
   건조The organic layer is dried with Na2SO4
5. 5
   기타the solvent is evaporated in vacuo
6. 6
   기타The residue is purified by HPLC (MeOH/H2O/TFA)

실험 절차

To 33.5 mg (120 μmol) 2-[4-(4-ethoxy-phenylethynyl)-phenyl]-1-methyl-ethylamine (I64) in 2.0 mL ACN are added 166 mg (1.20 mmol) K2CO3, a few crystals DMAP and finally 23.5 μL (0.18 mmol) 3-chloropivaloyl chloride (in 1.0 mL ACN). The reaction mixture is stirred at reflux for 6 h. The solvent is removed in vacuo and the residue is resolved EtOAc and washed with water (1×), sat. aq. NaHCO3 solution (2×) and again with water. The organic layer is dried with Na2SO4 and the solvent is evaporated in vacuo. The residue is purified by HPLC (MeOH/H2O/TFA).

출처