p-Toluenesulfonic acid monohydrate → p-Toluenesulfonic acid

Participants

Reaction Conditions

Reaction Steps

To a solution of above N1-(tert-butoxycarbonyl)-N2-(2-(trimethylsilyl)ethoxycarbonyl)-N2-(aminocarbonylmethyl)-(S)-3-cyclohexylpropane-1,2-diamine in ether (2 mL) was added TsOH.H2O (36.9 mg, 0.22 mmol) in ethanol (1 mL). The resulting solution was put on a rotatory vaporator, ether was removed in vacuum at rt, the bath temperature was raised to 60-65° C., and the mixture was heated in vacuo for 30 min to give (2S)-1-(N-(aminocarbonylmethyl)-N-(2-(trimethylsilyl)ethoxycarbonyl)amino)-3-cyclohexylpropyl-2-amine as a p-toluenesulfonic acid salt. MS ESI+ve m/z 358 (M+1).

Provenance & Evidence