反应详情

A mixture of 1.06 g (3.9 mmol) (1H-indol-5-yl)-(4-isopropyl-piperazin-1-yl)-methanone (intermediate 1); 0.484 g (4.3 mmol) KOtBu and 1.33 g (4.7 mmol) toluene-4-sulfonic acid 1-methyl-piperidin-3-ylmethyl ester (intermediate 6) in 20 mL THF was shaken at 60° C. for 3 h. After evaporation of all volatiles a mixture ethyl acetate was added and washed with water. The organic phase was dried with MgSO4 and evaporated to dryness. The residue was purified by column chromatography on silica eluting with a solvent mixture formed from DCM, methanol NEt3. The combined product fractions were evaporated to yield 1.44 g (91%) of the title compound as light yellow gum. MS(m/e): 383.5 (MH+).

1. customAfter evaporation of all volatiles a mixture ethyl acetate
2. additionwas added
3. washwashed with water
4. dry with materialThe organic phase was dried with MgSO4
5. customevaporated to dryness
6. customThe residue was purified by column chromatography on silica eluting with a solvent mixture
7. customformed from DCM, methanol NEt3
8. customThe combined product fractions were evaporated