반응 #65855

반응 방정식

product

5-Nitro-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

→

product

수율 71.2%

5-Amino-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

수율 71.2%

용매

tetrahydrofuran

hydrogen

반응 조건

후처리

1. 1
   여과After filtration
2. 2
   기타the solvent was removed
3. 3
   workup.DISTILLATIONthe residue was distilled under high vacuum

실험 절차

57.4 g of the product of Example 27 were dissolved in 400 ml of tetrahydrofuran and hydrogenated with hydrogen at 50 bar for 5 hours at 30° C. in the presence of 4 g of catalyst (palladium-on-charcoal, 10% by weight). After filtration, the solvent was removed and the residue was distilled under high vacuum to give 37 g of product (=63% of theory) with a boiling point of 83° C. at 0.07 mbar. 19F NMR: -59.0 and -84.6 ppm. 1H NMR: 2.98 ppm.

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