反应详情

A solution of 1,1-dimethylethyl (1-{2-[6-(methyloxy)-3-oxopyrido[2,3-b]pyrazin-4(3H)-yl]ethyl}-4-piperidinyl)carbamate (470 mg, 1.2 mmol) in DCM/trifluoroacetic acid (10 ml/10 ml) was stirred at rt for 30 minutes then evaporated to dryness. The residue was triturated with ether and then resultant solid dried in vacuo. The solid was dissolved in DCM/MeOH (20 ml/20 ml) and treated with MP-carbonate resin (2.3 mmol of carbonate per gram, 3 g, ca 8 mmol). After 1.5 hours the mixture was filtered, washing alternatively with small volumes of DCM and MeOH. The combined filtrates were evaporated affording a yellow oil (contaminated with particulate material from the resin). This residue was treated with 20% MeOH in DCM (20 ml) filtered and evaporated affording a yellow oil (350 mg, 100%).

1. customthen evaporated to dryness
2. customThe residue was triturated with ether
3. customresultant solid dried in vacuo
4. dissolutionThe solid was dissolved in DCM/MeOH (20 ml/20 ml)
5. filtrationAfter 1.5 hours the mixture was filtered
6. washwashing alternatively with small volumes of DCM and MeOH
7. customThe combined filtrates were evaporated
8. customaffording a yellow oil (
9. filtrationfiltered
10. customevaporated