反应详情

4-[2-(Azetidin-1-yl)ethyl]piperazine-1-carboxylic acid [6-(2-fluoro-4-nitrophenoxy)pyrimidin-4-yl]amide (110 mg) was dissolved in tetrahydrofuran (3 ml) and methanol (3 ml), and then 10% palladium carbon (53 mg) was added, followed by stirring under a hydrogen atmosphere for 16.5 hrs. The catalyst was filtered off and washed with methanol. The filtrate and washings were concentrated under reduced pressure to give a residue, which was then purified by silica gel column chromatography (Fuji Silysia NH, heptane: ethyl acetate:ethanol=95:5 to 90:10). Fractions containing the target compound were concentrated to provide a crude product of the titled compound (32.4 mg) as a yellow oil.

1. filtrationThe catalyst was filtered off
2. washwashed with methanol
3. concentrationThe filtrate and washings were concentrated under reduced pressure
4. customto give a residue, which
5. customwas then purified by silica gel column chromatography (Fuji Silysia NH, heptane: ethyl acetate:ethanol=95:5 to 90:10)
6. additionFractions containing the target compound
7. concentrationwere concentrated