Synthetic Route of 116861-31-5, These common heterocyclic compound, 116861-31-5, name is tert-Butyl (3-chloropropyl)carbamate, 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.
EXAMPLE 1 5-[(tert-butoxy)carbonyl]amino-2-ethoxycarbonyl-pentanoic acid ethyl ester (I: R1 =R2 =Et; R=–(CH2)3 –NHY; Y=Boc) Sodium metal (2.5 g, 0.1 mol) is dissolved in absolute ethyl alcohol (70 ml) while keeping the reaction mixture under nitrogen atmosphere. The temperature is then brought to 60 C. and malonic acid di-ethyl ester (35 g, 0.2 mol) is gradually dripped in. N-[(tert-butoxy)carbonyl]-3-chloro-propylamine (12.2 g, 0.1 mol) is gradually added, at room temperature, to the resulting solution. Stirring is continued at room temperature for 2 hours and then at the reflux temperature for 6 hours. The reaction mixture is poured into an ethyl acetate/water (1/1, v/v) mixture (400 ml) and the organic phase is recovered, washed several times with water and dried over MgSO4. The organic solvent is removed under vacuum (0.5 mBar) at 100 C., yielding a pale yellow oil (27.7 g, 87%), N.M.R. analysis of this product confirms the assigned structure.
The synthetic route of 116861-31-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Eniricerche S.p.A.; Sclavo S.p.A.; US4914226; (1990); A;,
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