反应详情

温度

60 °C

2 (56.970 g, 0.102 mol) was dissolved in 200 mL 1:1:EtOH:dioxane in a 1-L round-bottom flask, resulting in a dark orange, clear solution, to which a suspension of LiOH (7.315 g, 0.305 mol) in 75 mL water was added. The flask was fitted with a reflux condenser and magnetically stirred. The emulsion (containing undissolved LiOH) was heated to 60° C. for 12 h, and became a translucent, orange solution. The reaction mixture was filtered through a M glass frit, dissolved in 500 mL basic water, and washed with DCM (3×250 mL). The aqueous layer was acidifed with ˜80 mL conc. HCl, and the resulting white precipitate was filtered and washed with water. The solid was dried using house vacuum overnight, ground into a white powder, and dried on the vacuum line for 12 h (100%).

1. additionwas added
2. customThe flask was fitted with a reflux condenser
3. filtrationThe reaction mixture was filtered through a M glass frit
4. dissolutiondissolved in 500 mL basic water
5. washwashed with DCM (3×250 mL)
6. filtrationthe resulting white precipitate was filtered
7. washwashed with water
8. customThe solid was dried
9. customhouse vacuum overnight, ground
10. customdried on the vacuum line for 12 h (100%)