反应详情

A solution of 6-(4-ethylsulfonylpiperazin-1-yl)-3-methyl-pteridin-4-one (5 g, 14.78 mmol) in methanol (51.00 mL) was treated with sodium hydroxide (45.92 mL of 10% w/v, 114.8 mmol) and the reaction mixture stirred at RT overnight. The reaction mixture was concentrated in vacuo and the residue diluted with water and neutralised with formic acid. The resulting precipitate was filtered off and the filtrate acidified to pH4 by the addition of formic acid and extracted with dichloromethane. The combined organics were washed with brine, dried over MgSO4 and concentrated in vacuo to give the product as a bright yellow solid (4.66 g, 52% Yield). 1H NMR (400.0 MHz, CDCl3) d 1.45 (3H, t), 3.05 (2H, q), 3.54 (8H, m), 6.05 (2H, br s), 8.21 (1H, s) ppm; MS (ES+) 316

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionthe residue diluted with water and neutralised with formic acid
3. filtrationThe resulting precipitate was filtered off
4. additionthe filtrate acidified to pH4 by the addition of formic acid
5. extractionextracted with dichloromethane
6. washThe combined organics were washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo