反应详情

A mixture of 2-chloro-5-(5-isopropyl-2-methyl-phenoxymethyl)-4-methyl-6-piperazin-1-yl-pyrimidine trifluoroacetic acid salt (722 mg), 2-bromoacetamide (290 mg, 2.11 mmol) and potassium carbonate (871 mg, 6.30 mmol) in DMA (10 mL) is stirred at room temperature for 3 h. The reaction mixture is partitioned between EtOAc (30 mL) and water (10 mL), the organic layer is separated, washed with water (10 mL×2), brine (10 mL), dried over sodium sulfate, filtered and evaporated at reduced pressure to yield a yellow oil. Purification by chromatography on silica gel affords the title compound as a colorless oil that solidifies on standing. 1H NMR (CDCl3) δ=7.10 (d, 1H), 6.92 (br s, 1H), 6.82 (d, 1H), 6.74 (s, 1H), 5.54 (br s, 1H), 4.83 (s, 2H), 3.61, (m, 4H), 3.04 (s, 2H) 2.90 (m, 1H), 2.63 (m, 4H), 2.47 (s, 3H), 2.14 (s, 3H), 1.27 (d, 6H).

1. customThe reaction mixture is partitioned between EtOAc (30 mL) and water (10 mL)
2. customthe organic layer is separated
3. washwashed with water (10 mL×2), brine (10 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customevaporated at reduced pressure
7. customto yield a yellow oil
8. customPurification by chromatography on silica gel