反应详情

Alternatively Compound 13 was obtained by the following procedure: 5-methyl-2-(pyrimidin-2-yl)benzoic acid (428 mg, 2 mmol; prepared according to WO 2008147518), intermediate 34 (500 mg, 2 mmol) and DIPEA (0.65 ml) were dissolved in DCM (5 ml) at 0° C., then T3P (50% in DCM, 1.5 g) was added. The mixture is stirred at reflux for 8 hours then at RT overnight. The reaction was washed with NaOH 1M and water, dried (Na2SO4) and evaporated. The crude was purified by silica gel column chromatography (DCM to DCM/MeOH=95/05). 180 mg of the desired compound were isolated.

1. temperatureat reflux for 8 hours
2. customat RT
3. customovernight
4. washThe reaction was washed with NaOH 1M and water
5. dry with materialdried (Na2SO4)
6. customevaporated
7. customThe crude was purified by silica gel column chromatography (DCM to DCM/MeOH=95/05)