反应详情

To a solution of 3-ethyl-3-(3-nitrophenyl)-1,5-pentanediol (Preparation 61, 661 mg, 2.27 mmol) in toluene (24 ml) was added triethylamine (0.76 ml, 5.43 mmol) followed by methanesulfonyl chloride (0.42 ml, 5.4 mmol). The reaction mixture was stirred at room temperature under nitrogen for 18 h. The reaction mixture was poured onto water (10 ml), the phases were separated and the aqueous layer was extracted with dichloromethane (10 ml). The combined extracts were dried (MgSO4), filtered and concentrated in vacuo to give the title compound as an oil which was used without further purification (850 mg, 81% crude yield).

1. additionThe reaction mixture was poured onto water (10 ml)
2. customthe phases were separated
3. extractionthe aqueous layer was extracted with dichloromethane (10 ml)
4. dry with materialThe combined extracts were dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo