反应详情

At RT, 12 μl (68 μmol) of N,N-diisopropylethylamine and then 11 mg (65 μmol) of 4-nitrophenyl formate were added to a solution of 38 mg (62 μmol) of the compound of Example 53A in 1 ml of THF, and the mixture was stirred at RT. After 1 h, another 10 mg (62 μmol) of 4-nitrophenyl formate were added and stirring of the reaction mixture was continued overnight. Since LC/MS analysis indicated additional formation of an O-formylated byproduct, 248 μl of a 1 N solution of lithium hydroxide in water were added to the reaction mixture. After 1 h, the mixture was acidified with 1 N hydrochloric acid and separated by preparative HPLC [Method 8]. This gave 30 mg (81% of theory) of the title compound as a diastereomer mixture.

1. stirringstirring of the reaction mixture
2. waitwas continued overnight
3. additionwere added to the reaction mixture
4. waitAfter 1 h
5. customseparated by preparative HPLC [Method 8]