反应详情

温度

60 °C

A solution of 9-bromo-1-nonanol (0.314 g) in MeCN (3 mL) was added to solution of (5-methylthiophen-2-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone trifluoroacetate (example 9, step b) (0.263 g) and triethylamine (0.261 mL) in MeCN (7 mL). The resulting mixture was stirred at 60° C. under argon for 16 h. After cooling to RT the solvent was removed in vacuo. The residue was taken up in DCM, washed with brine (×2), dried over sodium sulphate, filtered and evaporated in vacuo. The white solid was purified by silica gel chromatography eluting with 0-10% MeOH in DCM to give the subtitled compound as a white solid. Yield 0.352 g.

1. temperatureAfter cooling to RT the solvent
2. customwas removed in vacuo
3. washwashed with brine (×2)
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. customevaporated in vacuo
7. customThe white solid was purified by silica gel chromatography
8. washeluting with 0-10% MeOH in DCM