反应详情

The crude acid 1b (310 mg, 0.95 mmol) was dissolved in 5 ml of dichloromethane. HOPO (111 mg, 1 mmol) and MEI (0.159 ml, 1.14 mmol) were added successively. The mixture was stirred for 30 minutes, then TMSONH2 (0.233 ml, 1.9 mmol) was added. After one hour another portion of TMSONH2 (0.233 ml, 1.9 mmol) was added and stirring continued over night. The reaction mixture was filtered (solid contained mostly HOPO) diluted with 20 ml of dichloromethane and extracted twice with 2N-HCl and brine, dried over anhydrous sodium sulfate and evaporated. The crude solid (237 mg, 73%) was purified by preparative HPLC (methanol/water=1/1). Yield: 100 mg (31%).

1. stirringstirring
2. waitcontinued over night
3. filtrationThe reaction mixture was filtered (solid
4. additiondiluted with 20 ml of dichloromethane
5. extractionextracted twice with 2N-HCl and brine
6. dry with materialdried over anhydrous sodium sulfate
7. customevaporated
8. customThe crude solid (237 mg, 73%) was purified by preparative HPLC (methanol/water=1/1)