反応 #2338

反応方程式

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

4-chloropyridine hydrochloride

triethylamine

→

title compound

収率 40.7%

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

収率 40.7%

溶媒

water

dioxan

反応条件

後処理

1. 1
   その他evaporated to dryness
2. 2
   その他The residue was triturated with water (2 ml)
3. 3
   ろ過filtered
4. 4
   その他The solid thus obtained
5. 5
   その他was recrystallised from water

実験手順

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%.

出典