反应详情

Magnesium metal (0.095 g, 3.91 mmol) was activated using a crystal of iodine prior to addition of THF (1 mL). 1-Bromo-4-methoxybenzene (0.400 g, 2.139 mmol) was added, and the reaction was left without stirring for 5 minutes after which initiation was observed. Additional THF (15 mL) was added and the mixture was stirred for 2 hours. (S,E)-2-Methyl-N-((3-(trifluoromethyl)pyridin-2-yl)methylene)propane-2-sulfinamide (0.500 g, 1.797 mmol) was added, and the mixture was stirred for 10 minutes. The reaction was quenched by addition of saturated aqueous NH4Cl (10 mL). H2O (100 mL) and EtOAc (150 mL) were added, and the phases mixed and separated. The organic layer was dried with MgSO4 and evaporated to dryness under reduced pressure. Purification using silica chromatography (hexane to EtOAc gradient) gave (S)—N—((S)-(4-methoxyphenyl)-(3-(trifluoromethyl)pyridin-2-yl)methyl)-2-methylpropane-2-sulfinamide.

1. waitthe reaction was left
2. stirringthe mixture was stirred for 2 hours
3. stirringthe mixture was stirred for 10 minutes
4. customThe reaction was quenched by addition of saturated aqueous NH4Cl (10 mL)
5. additionH2O (100 mL) and EtOAc (150 mL) were added
6. additionthe phases mixed
7. customseparated
8. dry with materialThe organic layer was dried with MgSO4
9. customevaporated to dryness under reduced pressure
10. customPurification