反应详情

温度

45 °C

To a 10 L reaction were charged under N2, i-PrOH (3.5 L), H2O (3.5 L), 3-7 (1.0 equiv, 0.97 mol, 350 g), potassium fluoride mono hydrate (290 g, 3.0 eq, 3.0 mol) and 35 g of 20% Pd(OH)2/C (10% v/w). After evacuated/refilled with hydrogen three times, the mixture was warmed to 40-50° C. and vigorously stirred at that temperature under 1 atmosphere of hydrogen. After 18 hours, LC/MS indicated <1% of starting material 3-7 remained. The mixture was purged with N2 for 20 min, cooled to 22° C., and filtered. Both the wet cake and filtrate contained the product and processed separately.

1. customTo a 10 L reaction
2. additionwere charged under N2
3. customThe mixture was purged with N2 for 20 min
4. temperaturecooled to 22° C.
5. filtrationfiltered