反应详情

温度

55 °C

A solution of propargyl alcohol (2.11 Kg, 37.7 mol) in toluene (32.48 L) was degassed and heated to 55° C. The solution of di-prop-2-ynyl-carbamic acid benzyl ester (4.06 Kg, 17.86 mol, step 6) in toluene and Wilkinsons catalyst (0.162 Kg) were added in 10 equal portions such that temperature <65° C. (the exotherm was allowed to subside before the next addition was made). The solution was then stirred at 55° C. for 1 h and then cooled to 20° C. DCM (8.12 L) was added and the mixture was concentrated to a small volume. Toluene (8 L) was added and the solution evaporated to constant weight giving the title compound 5.72 Kg (113%).

1. additionwere added in 10 equal portions such that temperature <65° C. (the exotherm
2. additionto subside before the next addition
3. temperaturecooled to 20° C
4. concentrationthe mixture was concentrated to a small volume
5. additionToluene (8 L) was added
6. customthe solution evaporated to constant weight