[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][CH2:6][NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11].[S:15](=[O:19])(=[O:18])(N)[NH2:16]>O1CCOCC1.C(OC(C)C)(C)C>[C:10]([O:9][C:8](=[O:14])[NH:7][CH2:6][CH2:5][CH2:4][CH2:3][N:2]([S:15]([NH2:16])(=[O:19])=[O:18])[CH3:1])([CH3:11])([CH3:13])[CH3:12]A mixture of tert-butyl 4-(methylamino)butylcarbamate (4 g, 19.77 mmoles) and sulfuric diamide (7.6 g, 4 eq) in dioxane (10 mL) was heated at 100° C. in a microwave oven during 30 minutes. The RM was then concentrated in vacuo, and DCM was added. The resulting white precipitate of sulfuric diamide in excess was filtered off, and the filtrate was successively washed with diluted HCl, then brine, dried over magnesium sulfate, filtered and concentrated. Trituration in diisopropyl ether afforded 3.55 g (64% yield) of tert-butyl 4-(methyl(sulfamoyl)amino)butylcarbamate 10b as a white solid; m/z 282 [M+H]+.
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