反应详情

90 mg of the tosylate from example 4 in 8 ml NMP were treated with 0.62 ml 2 M dimethylamine in THF and stirred at room temperature for 3 d. The mixture was heated to 50° C. for 4 hrs, then to 65° C. for another 2 hrs. Stirring was continued at 45° C. over night. Separation by HPLC-MS yielded crude product contaminated by NMP, which was further purified by dissolving in CHCl3 and washing with water.

1. temperatureThe mixture was heated to 50° C. for 4 hrs
2. waitto 65° C. for another 2 hrs
3. stirringStirring
4. waitwas continued at 45° C. over night
5. customSeparation by HPLC-MS
6. customyielded crude product
7. customwas further purified
8. dissolutionby dissolving in CHCl3
9. washwashing with water