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温度

0 °C

A solution of tert-butyl azetidin-3-ylcarbamate (1.00 g, 5.81 mmol) [Ark Pharma, AK26432] in tetrahydrofuran (50 mL) was treated with triethylamine (1.6 mL, 11.6 mmol) followed by N,N-dimethylformamide (15 mL) and cooled to 0° C. The reaction mixture was treated with acetyl chloride (495 μL, 6.97 mmol) and stirred overnight at room temperature. The reaction mixture was diluted with ether and washed with water and brine, dried over magnesium sulfate, filtered, and concentrated give a crude residue that was used immediately without purification. The intermediate azetidine was diluted with methylene chloride (30 mL), treated with 4.0 M hydrogen chloride in dioxane (22.0 mL, 88.0 mmol), and stirred at rt for 30 min. The reaction mixture was diluted with ether and the precipitated solid was collected by filtration in order to give the desired product (550 mg, 63%) as a HCl salt. LCMS calculated for C5H11N2O (M+H)+: m/z=115.1; found: 115.2.

1. washwashed with water and brine
2. dry with materialdried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customgive a crude residue that
6. customwas used immediately without purification
7. additionThe intermediate azetidine was diluted with methylene chloride (30 mL)
8. stirringstirred at rt for 30 min
9. filtrationthe precipitated solid was collected by filtration in order