反应详情

4-(4-Isopropyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-5′-yl)phenol (0.15 g, 0.404 mmol) was dissolved in DMF (4 mL) in a 5 mL microwave vial. NaH (0.039 g, 1.62 mmol) was added slowly and the mixture was stirred at rt for 30 min. Chloro-N,N-dimethylacetamide (0.147 g, 1.21 mmol) was added and the reaction mixture was heated for 2.5 h at 130° C. in a microwave oven. The reaction mixture was evaporated in vacuo and the residue was redissolved in a mixture of DCM and water. The phases were separated and the aqueous phase was extracted with DCM (2×25 mL). The combined organic extracts were evaporated, redissolved in MeOH and purified by preparative HPLC Method B. This afforded an oil which was treated with HCl in diethyl ether to give a solid material. Recrystallization from acetone and MeOH afforded 75 mg (41%) of the title compound.

1. temperaturethe reaction mixture was heated for 2.5 h at 130° C. in a microwave oven
2. customThe reaction mixture was evaporated in vacuo
3. dissolutionthe residue was redissolved in a mixture of DCM and water
4. customThe phases were separated
5. extractionthe aqueous phase was extracted with DCM (2×25 mL)
6. customThe combined organic extracts were evaporated
7. dissolutionredissolved in MeOH
8. custompurified by preparative HPLC Method B
9. customThis afforded an oil which
10. customto give a solid material
11. customRecrystallization from acetone and MeOH