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Procedure for preparation of 3-(benzyloxy)azetidine hydrochloride 24:; tert-butyl 3-(benzyloxy)azetidine-l-carboxylate 23 (1.0 gm) was taken into a round bottomed flask and was added methanolic-HCl (15 mL, 20percent) and was stirred for lh at room temperature. After completion of the reaction (monitored by TLC), the solvent was removed under vacuum to get a white solid as a crude product. The crude product was washed with ethyl acetate repeatedly and then dried well to obtain compound 24 as a white solid (92percent) and was used further without purification.
92%
With hydrogenchloride In methanol at 20℃; for 1 h;
Procedure for preparation of 3-(benzyloxy)azetidine hydrochloride 24 tert-butyl 3-(benzyloxy)azetidine-1-carboxylate 23 (1.0 μm) was taken into a round bottomed flask and was added methanolic-HCl (15 mL, 20percent) and was stirred for 1 h at room temperature. After completion of the reaction (monitored by TLC), the solvent was removed under vacuum to get a white solid as a crude product. The crude product was washed with ethyl acetate repeatedly and then dried well to obtain compound 24 as a white solid (92percent) and was used further without purification.
Procedure for preparation of 3-(benzyloxy)azetidine hydrochloride 24:; tert-butyl 3-(benzyloxy)azetidine-l-carboxylate 23 (1.0 gm) was taken into a round bottomed flask and was added methanolic-HCl (15 mL, 20%) and was stirred for lh at room temperature. After completion of the reaction (monitored by TLC), the solvent was removed under vacuum to get a white solid as a crude product. The crude product was washed with ethyl acetate repeatedly and then dried well to obtain compound 24 as a white solid (92%) and was used further without purification.
92%
With hydrogenchloride; In methanol; at 20℃; for 1h;
Procedure for preparation of 3-(benzyloxy)azetidine hydrochloride 24 tert-butyl 3-(benzyloxy)azetidine-1-carboxylate 23 (1.0 mum) was taken into a round bottomed flask and was added methanolic-HCl (15 mL, 20%) and was stirred for 1 h at room temperature. After completion of the reaction (monitored by TLC), the solvent was removed under vacuum to get a white solid as a crude product. The crude product was washed with ethyl acetate repeatedly and then dried well to obtain compound 24 as a white solid (92%) and was used further without purification.
With hydrogenchloride; In ethyl acetate; at 20℃; for 6h;
Compound llA was treated with 25 mL EA solution of HCl (1 M) and the mixture wasstirred at rt for 6 hrs. The solvent was concentrated in vacuo to give about 410 mg of crude 3-benzyloxyazetidine (Compound llB) as a colorless oil which was used directly in the next step.MS: calc'd 164 (M+Ht, measured 164 (M+Ht.
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