反应详情

温度

-30 °C

120 ml of anhydrous THF are cooled to −5° C. and 36 ml of 3M methylmagnesium bromide in ether are added. The mixture is cooled to −30° C. and then 15 g of 7-isopropyl-2-methyl-1H-indole are added dropwise. The mixture is left stirring for 1 hour between −20° C. and −30° C. and then 30.9 g of 2,3-dichlorobenzoyl chloride, dissolved in 120 ml of THF, are added dropwise. The medium is left to return to AT and is then poured onto 300 ml of a saturated NH4Cl solution. Separation is carried out by settling, the organic layer is evaporated and then the residue is taken up in DCM. The organic phase is washed with a saturated NaCl solution and then it is dried and evaporated. The residue is chromatographed on silica while eluting with an AcOEt/cyclohexane (3/7, v/v) mixture.

1. waitThe mixture is left
2. additionare added dropwise
3. waitThe medium is left
4. customSeparation
5. customthe organic layer is evaporated
6. washThe organic phase is washed with a saturated NaCl solution
7. customit is dried
8. customevaporated
9. customThe residue is chromatographed on silica
10. washwhile eluting with an AcOEt/cyclohexane (3/7