反应详情

温度

100 °C

To a solution of 5-(2-methanesulfonyloxy-ethyl)-2-methyl-1H-indole-3-carboxylic acid benzyl ester (360 mg, 0.93 mmol, Example 56, Step D) in dioxane (10 mL) was added diisobutylamine (1.62 mL, 9.3 mmol). The mixture was stirred at 100° C. overnight and then partitioned between methylene chloride and water. The organic phase was washed with water and brine, dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo to give a solid residue, which was purified by chromatography (20% ethyl acetate in hexanes) to give 303 mg (77%) of the desired product as a white solid: mp 134-135° C.; MS(APCI+): m/z 421.3 (MH+); Anal. Calcd for C27H36N2O2: C, 77.10; H, 8.63; N, 6.66. Found: C, 76.94; H, 8.75; N, 6.55.

1. custompartitioned between methylene chloride and water
2. washThe organic phase was washed with water and brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo
6. customto give a solid residue, which
7. customwas purified by chromatography (20% ethyl acetate in hexanes)