反应详情

To a stirred solution of 27.8 g of 4-cyclopropyl-4-hydroxy-1-octyne (Example 190) and 33.3 g of imidazole in 130 ml of dimethylformamide at 5° C. is added 24 ml of chlorotrimethylsilane during 5 minutes. The solution is stirred at ambient temperature for 17 hours and then partitioned with 600 ml of hexane and 250 ml of ice water. The hexane phase is separated and washed successively with water and brine. The solution is dried over magnesium sulfate and evaporated to give a liquid, pmr spectrum (CDCl3): δ 0.12 (singlet, trimethylsiloxy group), 2.02 (triplet, HC≡C), and 2.45 (doublet, C≡CH2).

1. custompartitioned with 600 ml of hexane and 250 ml of ice water
2. customThe hexane phase is separated
3. washwashed successively with water and brine
4. dry with materialThe solution is dried over magnesium sulfate
5. customevaporated
6. customto give a liquid, pmr spectrum (CDCl3)