反应详情

A 3-L reaction flask equipped with a cooling bath, air stirrer, and thermometer probe is charged with 5-(4-Chloro-thiophen-2-yl)-1-methyl-1H-[1,2,4]triazole (105.3 g, 0.527 moles), ACN (1053 mL) and HOAc (105 mL) to form a solution. NBS (103.2 g, 0.580 moles) is added portion-wise over 30-60 minutes while maintaining the temperature at ≦31° C. After stirring for 1 hour2, GC analysis indicated reaction completion. The reaction mixture is poured into de-ionized H2O (2.1 L, 20 vol), stirred for 30 minutes, filtered, and washed with de-ionized H2O (2×1 L). The product is dried in a vacuum oven at 45° C. overnight to give the title compound as a pale yellow solid (123.0 g, 83.8%; 96.6% area-% by GC). 2 The reaction temperature decreased after 1 hour to 26.7° C.

1. customequipped with a cooling bath, air stirrer
2. customto form a solution
3. temperaturewhile maintaining the temperature at ≦31° C
4. customreaction completion
5. stirringstirred for 30 minutes
6. filtrationfiltered
7. washwashed with de-ionized H2O (2×1 L)
8. customThe product is dried in a vacuum oven at 45° C. overnight