反应详情

7-2 (2.0 g, 15.4 mmol) and 1 equivalent of sodium hydride (0.62 g, 15.4 mmol) were suspended in THF and stirred for 20 minutes before adding 2-chloro-1,3-thiazole-5-carbonitrile 2-2 (2.23 g, 15.4 mmol) and the other equivalent sodium hydride simultaneously. The reaction was refluxed for 1.5 hours, cooled, quenched with methanol and water, evaporated to dryness and partitioned between methylene chloride, methanol and water. The aqueous layer was evaporated to dryness and purified on a silica column (DCM to 9:1:0.1 DCM:MeOH:NH4OH) to afford 35-1. 1H-NMR (CD3OD): 8.75(s, 1H); 8.10(s, 1H); 7.09(s, 1H).

1. temperatureThe reaction was refluxed for 1.5 hours
2. temperaturecooled
3. customquenched with methanol and water
4. customevaporated to dryness
5. custompartitioned between methylene chloride, methanol and water
6. customThe aqueous layer was evaporated to dryness
7. custompurified on a silica column (DCM to 9:1:0.1 DCM:MeOH:NH4OH)
8. customto afford 35-1