Electric Literature of 85006-25-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 85006-25-3 name is tert-Butyl (tert-butoxycarbonyl)oxycarbamate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Preparation 2 [tert-Butoxycarbonyl-[(4-methoxyphenyl)methyl]amino] tert-butyl carbonate A 20 L reactor, under nitrogen is charged with (tert-butoxycarbonylamino) tert- butyl carbonate (812.9 g, 3.48 mol), dimethylformamide (4.4 L), potassium carbonate (626.5 g, 4.52 mol) and l -(chloromethyl)-4-methoxy -benzene (462 mL, 2.56 mol). The mixture is stirred at 40 C overnight. lH NMR analysis shows incomplete reaction. Additional potassium carbonate (626.5 g, 4.52 mol) is added and the mixture is stirred at 40 C. lH NMR analysis after 48 hours shows the reaction is still incomplete. Additional potassium carbonate (482 g, 3.49 mol) is added and the mixture is stirred at 40 C. lH NMR analysis after overnight reaction shows complete reaction with no starting materials remaining. Water (5 L) and MTBE (5 L) are added and the layers are separated. The organic layer is washed with water (3×3 L), dried over sodium sulphate, and concentrated to give the title compound (1.21 Kg, 98%). 1H NMR (d6-DMSO) delta 7.20 (d, J= 8.3 Hz, 2H), 6.91 (d, J= 8.3 Hz, 2H), 3.73 (s, 2H), 3.35 (s, 3H), 1.41 (s, 18H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl (tert-butoxycarbonyl)oxycarbamate, and friends who are interested can also refer to it.
Reference:
Patent; ELI LILLY AND COMPANY; MARTIN, Fionna Mitchell; WO2015/138208; (2015); A1;,
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