These common heterocyclic compound, 5616-81-9, name is tert-Butyl 2-(methylamino)acetate, 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. Formula: C7H15NO2
Bromoacetyl bromide (3.56 g, 17.6 mmol,1.55 ml, 1.5 equivalent), dry CH2C12 (50 ml) and K3P04 (6.41 g, 30.2 mmol, 2.5 equ.) was mixed in a flask of 250 ml under N2 atmosphere. Sarcosine tert-butyl ester (1.7 g, 11.7 mmol, 1.0 equivalent) was dissolved in dry CH2C12 (20 ml) and was added dropwise to dichloromethane solution of bromoacetyl bromide at 0 C in 30 minutes, then the reaction mixture was stirred for additional 12 hours at room temperature under N2 atmosphere before the aqueous HC1 solution (0.5 M, 30 ml) was added to the reaction mixture. After the addition of RC1 solution, the reaction mixture was stirred for additional 5 minutes, then the two phases were separated using a separatory funnel. The aqueous phase was washed with CH2C12 (1 x 15 ml) and then the unified organic phases were washed with KHCO3 solution (2 x 30 ml, 10 mlm%) and saturated NaC1 solution(1 x 30 ml). The organic phase was dried with MgSO4, then dichioromethane was evaporated at reduced pressure, and the crude product was stored at -20 C until further use. Yield: 2.01 g (65%). ?H NMR [360 MHz, CDCl3] oe 1.6 (9H, s, CR3) 2.8 (3H, s, CR3), 4.01 (2H, s, CH2), 4.4 (2H, s, CR2)
The synthetic route of tert-Butyl 2-(methylamino)acetate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; DEBRECENI EGYETEM; BOTAR, Richard; GARDA, Zoltan; FODOR, Tamas; KALMAN, Ferenc Krisztian; NAGY, Viktoria; TIRCSO, Gyula; TOTH, Imre; (44 pag.)WO2017/89847; (2017); A1;,
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