Dichloromethane → HCID 178484833, compound

Participants

Reaction Steps

254 μl of methanesulfonyl chloride was added to a methylene chloride solution containing 500 mg of N-tert-butoxycarbonyl-N′-methyl-trans-1,4-cyclohexanediamine (Reference Example 10-14 (1)) and 763 μl of triethylamine, and the mixture was stirred at room temperature for 14 hours. To the reaction mixture were added water, followed by an aqueous saturated sodium hydrogencarbonate solution, and the mixture was extracted with ethyl acetate. The extract was-washed with an aqueous saturated sodium hydrogencarbonate, water and brine, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The obtained residue was suspended in diisopropyl ether, and collected by filtration to obtain N-tert-butoxycarbonyl-N′-methyl-N′-methylsulfonyl-trans-1,4-cyclohexanediamine. Subsequently, this compound was treaded with hydrochloric acid to obtain N-methyl-N-methylsulfonyl-trans-1,4-cyclohexanediamine (Reference Example 10-18 in Table 11).

Provenance & Evidence