反应详情

温度

0 °C

A 5.76 g (0.072 mol) 50% aqueous solution of sodium hydroxide was added slowly to a solution of 8.6 g (0.036 mol) N-cyclopentyl bromomethanesulfonamide, 8.6 g (0.036 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride, and about 0.1 g benzyltriethyl ammonium chloride in 200 mol dichloromethane cooled to 0° C with an ice bath. The reaction mixture was then stirred at 0° C for 2 hours, washed with water, dried over magnesium sulfate and evaporated to give a brown oil. The oil was chromatography over silica gel with dichloromethane/petroleum-ether elution to give 5.5 g (35% yield) of the product, as a grey solid, m.p. 59°-60° C. The elemental analysis for the product is tabulated in Table I under compound No. 9.

1. washwashed with water
2. dry with materialdried over magnesium sulfate
3. customevaporated
4. customto give a brown oil
5. washwith dichloromethane/petroleum-ether elution