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ChemicalBook CAS DataBase List 1-N-Boc-3-methylbutane-1,3-diamine-HCl
880100-30-1

1-N-Boc-3-methylbutane-1,3-diamine-HCl synthesis

1synthesis methods
181646-38-8 Synthesis
Carbamic acid, (1,1-dimethyl-3-oxopropyl)-, 1,1-dimethylethyl ester (9CI)

181646-38-8
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Yield:880100-30-1 96%

Reaction Conditions:

with ammonia;hydrogen;Raney nickel in ethanol at 20; under 2250.23 Torr;

Steps:



23.6 g (117 mmol) tert-butyl (1,1-dimethyl-3-oxo-propyl)-carbamate in 700 mL ethanolic ammonia solution are treated in the presence of 3.5 g Raney nickel at ambient temperature with 3 bar hydrogen pressure until no more educt can be detected by thin layer chromatography. The catalyst is filtered off and the solvent eliminated by distillation. Dark green oil. Yield: 22.7 g (96%); mass spectroscopy: [M+H]+=203.

References:

US2006/63817,2006,A1 Location in patent:Page/Page column 8