반응 #2338

반응 방정식

methyl 4-[2-(piperazin-2-one-1-yl)acetyl]-phenoxyacetate

4-chloropyridine hydrochloride

triethylamine

→

title compound

수율 40.7%

4-[2-[4-(4-pyridyl)piperazin-2-one-1-yl]acetyl]-phenoxyacetic acid monohydrochloride

수율 40.7%

용매

water

dioxan

반응 조건

후처리

1. 1
   기타evaporated to dryness
2. 2
   기타The residue was triturated with water (2 ml)
3. 3
   여과filtered
4. 4
   기타The solid thus obtained
5. 5
   기타was recrystallised from water

실험 절차

A solution of methyl 4-[2-(piperazin-2-one-1-yl)acetyl]-phenoxyacetate (0.347 g), 4-chloropyridine hydrochloride (0.19 g) and triethylamine (0.178 g) in water (8 ml) and dioxan (1 ml) was heated on a steam bath for 2 hours and then evaporated to dryness. The residue was triturated with water (2 ml) and filtered. The solid thus obtained was recrystallised from water to give the title compound (0.187 g), m.p. 275°-277° C.; NMR(d6DMSO δ 8.33(2H,d), 8.0(2H,d), 7.21(2H,d), 7.1(2H,d), 4.97(2H,s), 4.81(2H,s), 3.94(2H,m), 3.59(2H,m); m/e 370(H+H)+ ; calculated for C19H20N3O5Cl. 0.75 H2O: C, 54.4; H, 5.0; N, 10.0. Found: C, 54.5; H, 5.3; N, 9.5%.

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