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924964-23-8

DI-TERT-BUTYL 2-CYANOPIPERAZINE-1,4-DICARBOXYLATE synthesis

3synthesis methods
di-tert-butyl 2-carbamoylpiperazine-1,4-dicarboxylate

927883-45-2
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DI-TERT-BUTYL 2-CYANOPIPERAZINE-1,4-DICARBOXYLATE

924964-23-8
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Yield:924964-23-8 89.5%

Reaction Conditions:

with 1,3,5-trichloro-2,4,6-triazine in N,N-dimethyl-formamide at 20; for 1 h;

Steps:

2.1

2,4,6-Trichloro-1,3,5-triazine (2.12 g, 11.52 mmol) and DMF (15 mL) were added and the resulting mixture was stirred at room temperature for 1 h prior to quenching with water and extraction with ethyl acetate. The organic layer was washed with water (3*) and brine (1*), dried over magnesium sulfate, and evaporated in vacuo to give the title compound (5.36 g, 89.5%). 1H NMR (300 MHz, CDCl3): δ (ppm)=5.08 (br m, 1H); 4.36 (br m, 1H); 4.25 (br m, 1H); 3.95 (br d, 1H); 3.06 (br t, 2H); 2.80 (br m, 1H); 1.51 (s, 18H).

References:

US2007/49578,2007,A1 Location in patent:Page/Page column 22