反应详情

To a solution of N,N′-di-Boc-2-hydroxy-1,3-diaminopropane (13.19 g, 45.4 mmol) and triethylamine (1.5 eq, 9.5 ml, 68.1 mmol) in dry 50 ml CH2Cl2 was added dropwise a solution of methanesulfonyl chloride (1.5 eq, 5.25 ml, 68 mmol) in dry 15 ml CH2Cl2 over a period of 1 h at 0° C. with stirring under nitrogen. After the addition, the reaction was stirred overnight at room temperature. Water was slowly added to quench the reaction; the organic layer was separated and then washed with water (5×15 ml) and dried over Na2SO4 and evaporated to give white solid. Recrystallization from hot acetone and cyclohexane gave 10.36 g (62%) white solid. M.p.=127° C.

1. additionAfter the addition
2. stirringthe reaction was stirred overnight at room temperature
3. customto quench
4. customthe reaction
5. customthe organic layer was separated
6. washwashed with water (5×15 ml)
7. dry with materialdried over Na2SO4
8. customevaporated
9. customto give white solid
10. customRecrystallization from hot acetone and cyclohexane