반응 #312986

반응 방정식

1-(diphenylmethyl)azetidin-3-yl methanesulfonate

chloroethylchloroformate

→

title compound

Azetidin-3-yl methanesulfonate hydrochloride

용매

dichloromethane

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 2.5 hours
3. 3
   농축The reaction mixture was then concentrated in vacuo
4. 4
   workup.DISSOLUTIONthe residue was re-dissolved in methanol (100 mL)
5. 5
   온도heated
6. 6
   온도under reflux for a further 2.5 hours
7. 7
   농축concentrated in vacuo

실험 절차

A mixture of 1-(diphenylmethyl)azetidin-3-yl methanesulfonate (WO 97/25322, p64), (20 g, 63 mmol) and chloroethylchloroformate (10 mL, 95 mmol) in dichloromethane (100 mL) was heated under reflux for 2.5 hours. The reaction mixture was then concentrated in vacuo and the residue was re-dissolved in methanol (100 mL) and heated under reflux for a further 2.5 hours. The mixture was then cooled to room temperature and concentrated in vacuo to afford the title compound as a white solid in quantitative yield, 9.6 g. 1H NMR(400 MHz, DMSO-d6) δ: 3.28(s, 3H), 4.06(m, 2H), 4.31(m, 2H), 5.34(m, 1H)

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