反应详情

To a suspension of 3.76 g. (0.02 mole) of 5-chloro-2-methoxynicotinic acid in 100 ml. of carbon tetrachloride, there were added 100 ml. of thionyl chloride in one portion and the resulting mixture was then refluxed on a steam bath for a period of 90 minutes. Upon completion of this step, the clear solution so obtained was cooled and then concentrated in vacuo at room temperature to afford a residual oil. The excess thionyl chloride present was next removed in the same manner as described in Preparation A for the production of 2-methoxynicotinoyl chloride, except that only 100 ml. of benzene was employed this time (i.e., during each purification step). The yield of pure 5-chloro-2-methoxynicotinoyl chloride, obtained as the residual product, was quantitative in this particular instance.

1. additionTo a suspension of 3.76 g
2. customUpon completion of this step, the clear solution so obtained
3. temperaturewas cooled
4. concentrationconcentrated in vacuo at room temperature
5. customto afford a residual oil
6. customThe excess thionyl chloride present was next removed in the same manner
7. customas described in Preparation A for the production of 2-methoxynicotinoyl chloride, except that only 100 ml
8. customduring each purification step)