反应详情

温度

50 °C

A solution of 1,1-dimethylethyl 4-({2-amino-5-[(1-methylethyl)oxy]phenyl}amino)-1-piperidinecarboxylate (D48, 470 mg, 1.34 mmol) in tetrahydrofuran (5 ml) was treated with N,N′-carbonyldiimidazole (322 mg, 2.01 mmol) and heated at 50° C. for 17 hrs. The mixture was concentrated under vacuum and the residue treated with Na2CO3 solution (10 ml) and extracted with ethyl acetate (2×20 ml). The combined extract was dried (MgSO4), concentrated under vacuum and the residue purified by chromatography on silica gel eluting with 5-60% ethyl acetate/60-80 petrol ether to afford the title compound as a dark orange oil (351 mg, 69%). M+−H=374.3.

1. concentrationThe mixture was concentrated under vacuum
2. additionthe residue treated with Na2CO3 solution (10 ml)
3. extractionextracted with ethyl acetate (2×20 ml)
4. extractionThe combined extract
5. dry with materialwas dried (MgSO4)
6. concentrationconcentrated under vacuum
7. customthe residue purified by chromatography on silica gel eluting with 5-60% ethyl acetate/60-80 petrol ether