反应 #4565
ord-67d46a104ad240b9a00c308bf07eb4cb
反应方程式
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度The resulting solution was cooled to ca 0° C.
- 2workup.STIRRINGThe reaction mixture was stirred at room temperature for 5 hours
- 3萃取it was extracted twice with 100 ml
- 4干燥The resulting toluene solution was dried
- 5浓缩it was concentrated in vacuo
- 6其他to give 32.6 g
实验过程
To 130 ml. of toluene was added, with stirring, 24.0 g. (0.165 mole) of 3-chloro-4-fluoroaniline and 13.5 ml. (0.166 mole) of pyridine. The resulting solution was cooled to ca 0° C. and 13.2 ml. (0.166 mole) of 2-chloroacetyl chloride was added. The reaction mixture was stirred at room temperature for 5 hours and then it was extracted twice with 100 ml. of 1N hydrochloric acid, followed by 100 ml. of saturated sodium chloride solution. The resulting toluene solution was dried using magnesium sulfate, and then it was concentrated in vacuo to give 32.6 g. (88% yield) of N-(2-chloroacetyl)-3-chloro-4-fluoroaniline.