反应详情

温度

0 °C

A mixture of (E)-9-methoxy-7,7-dimethylnon-8-en-1-ol and (Z)-9-methoxy-7,7-dimethylnon-8-en-1-ol (example 279, step d) (1.6 g) was dissolved in dichloromethane (15 mL) and triethylamine (1.33 mL) was added then the mixture was cooled to 0° C. in an ice bath under argon. Methanesulfonyl chloride (0.68 mL) was added dropwise over 5 minutes and the reaction mixture was stirred at 0° C. for 15 minutes and then at room temperature for 1 hour. The reaction mixture was washed with brine (2×30 mL), dried over magnesium sulfate, filtered and evaporated under vacuum to give the crude product. Purification was by silica gel chromatography, eluting with 0-100% ethyl acetate in cyclohexane to afford the subtitled compound as a colourless oil. Yield 1.2 g.

1. waitat room temperature for 1 hour
2. washThe reaction mixture was washed with brine (2×30 mL)
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated under vacuum
6. customto give the crude product
7. customPurification
8. washeluting with 0-100% ethyl acetate in cyclohexane