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ChemicalBook CAS DataBase List 1-N-Boc-5-oxo-1,4-diazepane

1-N-Boc-5-oxo-1,4-diazepane synthesis

6synthesis methods
-

Yield: 89%

Reaction Conditions:

in tetrahydrofuran at 10 - 20; for 2 h;

Steps:

5
Intermediate 5 :tert-butyl 5-oxo-l,4-diazepane-l-carboxylate; To a stirred solution of commercially available l,4-diazepan-5-one (3.3 g, 28.94 mmol) in THF cooled to 10°C, was added di-tert-butyl dicarbonate(9.5 g, 43.42 mmol) and the resultant reaction mixture was stirred at RT for 2 h. The reaction mixture was concentrated under reduced pressure and the resulting residue was washed with n-pentane (50 mL) to afford the title compound as a solid (5.5 g, 89%).:H NMR (300 MHz, DMSO) δ = 7.62 (s, 1H), 3.45-3.40 (m, 4H), 3.12-3.08 (m, 2H), 2.43-2.39 (m, 2H).

References:

LEO PHARMA A/S;NIELSEN, Simon, Feldbæk;GREVE, Daniel, Rodriguez;GRUE-SØRENSEN, Gunnar;RYTTERSGAARD, Carsten;SCHOU, Søren, Christian;SAMS, Anette, Graven WO2012/3829, 2012, A1 Location in patent:Page/Page column 59

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