4-perfluoroisopropylaniline synthesis
- Product Name:4-perfluoroisopropylaniline
- CAS Number:2396-17-0
- Molecular formula:C9H6F7N
- Molecular Weight:261.14
Yield:2396-17-0 99.6%
Reaction Conditions:
with sodium dithionite;tetra(n-butyl)ammonium hydrogensulfate;sodium hydrogencarbonate in tert-butyl methyl ether;water at 20; for 3 h;
Steps:
1 Example 1: Synthesis of intermediate 4-(heptafluoroisopropane)aniline:
Add 9.31g (100mmol) of aniline, 130mL of tert-butyl methyl ether and 130mL of water to a 500 round bottom flask, add 21.76g (125mmol) of sodium dithionite,17.70g (175mmol) sodium bicarbonate and 1.70g (5mmol) tetrabutyl ammonium hydrogen sulfate, 36.99g (125mmol) heptafluoroisopropyl iodide was added dropwise, magnetically stirred at room temperature for 3h, TLC (PE:EA=10:1) detects the completion of the reaction and stops the reaction. The organic phase is separated from the reaction solution, the aqueous phase is extracted with EA, the organic phases are combined, washed three times with saturated brine, dried with anhydrous magnesium sulfate, and evaporated to dryness. 26.00 g of reddish brown liquid was obtained, with a yield of 99.6%.
References:
CN112778192,2021,A Location in patent:Paragraph 0111-0115
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