反应详情

温度

110 °C

A mixture of crude 2-ethyl-6-methyl-isonicotinic acid N′-(1,1,2-trimethyl-1,1a,5,5a-tetrahydro-3-thia-cyclopropa[a]pentalene-4-carbonyl)-hydrazide (350 mg, ca. 0.5 mmol) and Burgess Reagent (385 mg, 1.62 mmol) in THF (5 mL) is heated at 110° C. for 3 min in a microwave oven. The mixture is diluted with EA (10 mL) and extracted with sat. aq. Na2CO3 (2×5 mL). The organic phase is dried (Na2SO4), filtered and evaporated to give crude product (50.9 mg) that is purified by HPLC to give 2-ethyl-6-methyl-4-[5-((1aS,5aR)-1,1,2-trimethyl-1,1a,5,5a-tetrahydro-3-thia-cyclopropa[a]pentalen-4-yl)-[1,3,4]oxadiazol-2-yl]-pyridine (16 mg) as a light yellow powder; LC-MS: tR=0.91 min, [M+1]=366.21.

1. extractionextracted with sat. aq. Na2CO3 (2×5 mL)
2. dry with materialThe organic phase is dried (Na2SO4)
3. filtrationfiltered
4. customevaporated
5. customto give crude product (50.9 mg) that
6. customis purified by HPLC