反应详情

温度

60 °C

A solution of 9-bromo-1-nonanol (0.335 g) in acetonitrile (3 mL) was added to a solution of (5-methylthiophen-3-yl)(1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)methanone (example 104, step b) (0.28 g) and triethylamine (0.278 mL) in acetonitrile (7 mL). The resulting mixture was stirred at 60° C. overnight. The reaction mixture was evaporated in vacuo and the residue was taken up into DCM (30 mL), washed with brine (2×15 mL), dried over sodium sulphate, filtered and evaporated in vacuo. Purification was by silica gel chromatography eluting with 0-10% methanol in dichloromethane to give the subtitled compound as a white solid. Yield 0.3 g.

1. customThe reaction mixture was evaporated in vacuo
2. washwashed with brine (2×15 mL)
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customevaporated in vacuo
6. customPurification
7. washeluting with 0-10% methanol in dichloromethane