反应详情

A mixture of 4-(4-isopropyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-5′-yl)phenylamine (0.34 g, 1.14 mmol), 3-chloro-1-propanesulfonyl chloride (0.20 g, 1.14 mmol) and TEA (0.12 g, 1.14 mmol) in DMF was stirred at rt for 1 h. NaH (0.055 g, 2.29 mmol) was added and stirring was continued for 5 h. The reaction mixture was transferred to a microwave vial (20 mL) and heated for 1000 s at 80° C. in a microwave oven. The reaction mixture was evaporated in vacuo and 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 in vacuo, redissolved in MeOH and purified by preparative HPLC Method B. This afforded 220 mg of a solid which was redissolved in MeOH and treated with HCl in diethyl ether. The volatiles were evaporated to give 126 mg (22%) of the title compound.

1. stirringstirring
2. waitwas continued for 5 h
3. temperatureheated for 1000 s at 80° C. in a microwave oven
4. customThe reaction mixture was evaporated in vacuo
5. dissolutionredissolved in a mixture of DCM and water
6. customThe phases were separated
7. extractionthe aqueous phase was extracted with DCM (2×25 mL)
8. customThe combined organic extracts were evaporated in vacuo
9. dissolutionredissolved in MeOH
10. custompurified by preparative HPLC Method B
11. dissolutionThis afforded 220 mg of a solid which was redissolved in MeOH
12. additiontreated with HCl in diethyl ether
13. customThe volatiles were evaporated