反应 #1885102
ord-d4afe6094a6a47cab4855c4d8e6fa711
反应方程式
5-aminobenzo[d]oxazol-2(3H)-one
2,4-dichloro-5-methylpyrimidine
MeOH
→
5-(2-Chloro-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one
收率 71.0%
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他Precipitate from reaction mixture
- 2过滤was collected by filtration
- 3洗涤washing with EtOAc (3 mL×2)
- 4其他was further dried in vacuo
实验过程
To a vial with 5-aminobenzo[d]oxazol-2(3H)-one (300.1 mg, 2.0 mmol) and 2,4-dichloro-5-methylpyrimidine (423.8 mg, 2.6 mmol), MeOH (8 mL) and H2O (2 mL) were added. The turbid mixture was stirred at room temperature for 64 h. Precipitate from reaction mixture was collected by filtration, washing with EtOAc (3 mL×2), and was further dried in vacuo. 5-(2-Chloro-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one was obtained as an off-white solid: 394 mg (71% yield); 1H NMR (300 MHz, DMSO) δ 11.68 (br s, 1H), 8.62 (s, 1H), 7.94 (d, J=0.8, 1H), 6.97 (d, J=2.0, 1H), 6.82 (d, J=8.1, 1H), 6.74 (dd, J=2.0, 8.1, 1H), 2.15 (s, 3H); LCMS (M+) m/z 277.10.