反应详情

To a solution of 2-chloro-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 (62.9 mg, 0.17 mmol), Fe(acac)3 (6 mg) and NMP (20 mg) in THF (5 mL) is added a solution of methylmagnesiumiodide in THF (3M, 0.51 mmol) and the mixture is stirred at rt for 15 h. The mixture is quenched with water (30 mL) and extracted with Et2O (2×50 mL). The organic extracts are dried (MgSO4), filtered and evaporated. The residue is purified by TLC (SiO2, EA-hexane) to give 2,6-dimethyl-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 (28 mg); LC-MS: tR=0.88 min, [M+1]=352.54.

1. customThe mixture is quenched with water (30 mL)
2. extractionextracted with Et2O (2×50 mL)
3. dry with materialThe organic extracts are dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue is purified by TLC (SiO2, EA-hexane)