반응 #159610

반응 방정식

azetidin-3-ol hydrochloride

trietylamine

methyl 2-chloropyridine-3-carboxylate

→

title compound ( D62 )

methyl 5-chloro-2-(3-hydroxyazetidin-1-yl)nicotinate

용매

methanol

반응 조건

후처리

1. 1
   기타The residue obtained
2. 2
   기타after solvent evaporation
3. 3
   기타was purified by SPE-Si cartridge (10 g)
4. 4
   세척eluting with a mixture cyclohexane/ethylacetate from 90/10 to 60/40
5. 5
   기타Collected fractions after solvent evaporation

실험 절차

To a solution of azetidin-3-ol hydrochloride (637 mg, 5.82 mmol, commercially available from Matrix Scientific #011272) and trietylamine (1.69 ml, 12.11 mmol) in methanol (10 ml), methyl 2-chloropyridine-3-carboxylate (1 g, 4.84 mmol) was added and the mixture stirred at 150° C. under microwave irradiation 10 min (2 cycles of 5 min each). The residue obtained after solvent evaporation was purified by SPE-Si cartridge (10 g) eluting with a mixture cyclohexane/ethylacetate from 90/10 to 60/40. Collected fractions after solvent evaporation afforded the title compound (D62) (D004/099/1) (800 mg)

출처