107017-73-2, A common heterocyclic compound, 107017-73-2, name is tert-Butyl (1-(hydroxymethyl)cyclopropyl)carbamate, molecular formula is C9H17NO3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
To a solution of tert-butyl (1-(hydroxymethyl)cyclopropyl)carbamate (3.5 g; 18.7 mmol)and imidazole (2.54 g; 37.4 mmol) in DCM (40 mL) was added TBDPSCl (4.11 mL;18.7 mmol). The reaction mixture was stirred for 4 h. Water (50 mL) and DCM (20 mL)were added. The two layers were separated and the aq. phase was extracted twice with25 DCM (2 x 25 mL).The evaporation residue was purified by CC (EA-Hept) to afford thetitle compound as a colourless oil (8.85 g; > 95% yield).1H NMR (d6-DMSO) o: 7.64-7.60 (m, 4H); 7.49-7.40 (m, 6H); 7.20 (s, 1H); 3.66 (s, 2H);1.36 (br. s, 9H); 1.00 (s, 9H); 0.71-0.65 (m, 2H); 0.64-0.60 (m, 2H).MS (ESI, m/z): 426.1 [M+H+] for CzsH3sN03Si; tR = 1.11 min.
The synthetic route of tert-Butyl (1-(hydroxymethyl)cyclopropyl)carbamate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; IDORSIA PHARMACEUTICALS LTD; DIETHELM, Stefan; MIRRE, Azely; PANCHAUD, Philippe; SCHMITT, Christine; SURIVET, Jean-Philippe; (99 pag.)WO2017/198647; (2017); A1;,
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