反应详情

The trans-N-boc-1,4-cyclohexanediamine (1.00 g, 4.67 mmol) was dissolved in DCM (50 mL). Next, TEA was added (1.301 mL, 9.33 mmol), followed by methanesulfonyl chloride (0.397 mL, 5.13 mmol). The reaction was allowed to stir at rt for 22 h. The reaction mixture was partitioned between DCM (100 mL) and water (25 mL). The phases were separated and the aqueous phase was extracted with DCM (50 mL). Combined organic layer was dried over MgSO4 for 20 h overnight. Filtered and evaporated to dryness to give the title compound of Step A as a solid (0.924 g). 1H NMR (400 MHz, DMSO-d6) δ ppm 3.32 (s, 8H), 2.89 (s, 3H), 1.83-1.91 (m, 1H), 1.70-1.78 (m, 1H), 1.37 (s, 9H).

1. additionNext, TEA was added (1.301 mL, 9.33 mmol)
2. customThe reaction mixture was partitioned between DCM (100 mL) and water (25 mL)
3. customThe phases were separated
4. extractionthe aqueous phase was extracted with DCM (50 mL)
5. dry with materialCombined organic layer was dried over MgSO4 for 20 h overnight
6. filtrationFiltered
7. customevaporated to dryness