反应详情

The product from Example 1C (3.67 g, 7.51 mmol) and 4-tert-butylaniline (11.86 ml, 75 mmol) in DMF (40 ml) was stirred under nitrogen at 50° C. for 4 h. The resulting mixture was diluted into ethyl acetate, treated with 1M HCl, stirred for 10 minutes and filtered to remove solids. The filtrate organic layer was washed twice with brine, dried with sodium sulfate, filtered and evaporated. The residue was purified by chromatography on silica gel eluting with ethyl acetate in hexane (5% to 30%) to give a solid. The solid was triturated in a minimal volume of 1:9 ethyl acetate/hexane to give a light yellow solid as a mixture of trans and cis isomers (1.21 g, 36%).

1. filtrationfiltered
2. customto remove solids
3. washThe filtrate organic layer was washed twice with brine
4. dry with materialdried with sodium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by chromatography on silica gel eluting with ethyl acetate in hexane (5% to 30%)
8. customto give a solid
9. customThe solid was triturated in a minimal volume of 1:9 ethyl acetate/hexane
10. customto give a light yellow solid
11. additionas a mixture of trans and cis isomers (1.21 g, 36%)