反应详情

A solution of racemic 1,1-dimethylethyl{(3R,4S)-1-[(3-fluoro-7-oxo-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-4-yl)methyl]-3-hydroxy-4-piperidinyl}carbamate (200 mg) in acetic acid (6 ml) was treated with a 4M solution of HCl in 1,4-dioxane (2 ml), stirred 2 h at room temperature and evaporated to dryness. A part solution/part suspension of this material in dichloromethane (8.5 ml) and methanol (1.5 ml) was treated with MP-carbonate resin (obtained from Argonaut Technologies) (1.2 g), stirred for 3 h, filtered and the resin washed well with 1:1 dichloromethane/methanol. The filtrate was evaporated and the residue chromatographed on silica gel, eluting with dichloromethane/methanol/0.88 ammonia (89:11:1.1) to give product (133 mg, 87%).

1. customevaporated to dryness
2. additionA part solution/part suspension of this material in dichloromethane (8.5 ml)
3. additionmethanol (1.5 ml) was treated with MP-carbonate resin (obtained from Argonaut Technologies) (1.2 g)
4. stirringstirred for 3 h
5. filtrationfiltered
6. washthe resin washed well with 1:1 dichloromethane/methanol
7. customThe filtrate was evaporated
8. customthe residue chromatographed on silica gel
9. washeluting with dichloromethane/methanol/0.88 ammonia (89:11:1.1)