反应详情

A mixture of 2-hydroxy-5-chlorobenzylamine (1.22 g, 4.77 mmol assuming the bisulfate salt), (BOC)2O (1.56 g, 7.16 mmol) and N-methylmorpholine (1.05 ml, 9.54 mmol) in DMF (10 ml) was stirred for 5 h at r.t. The reaction was partitioned between water and ethyl acetate and the organic layer was washed with 5% KHSO4 solution (2 times), sodium hydrogen carbonate solution and brine, dried (Na2SO4) and evaporated in vacuo to a solid. The crude product was recrystallized from ethyl acetate/hexanes (1:5, 12 ml) to give the title compound:

1. customThe reaction was partitioned between water and ethyl acetate
2. washthe organic layer was washed with 5% KHSO4 solution (2 times), sodium hydrogen carbonate solution and brine
3. dry with materialdried (Na2SO4)
4. customevaporated in vacuo to a solid
5. customThe crude product was recrystallized from ethyl acetate/hexanes (1:5, 12 ml)