반응 #517239

반응 방정식

1-(3-hydroxy-4-nitro-2,5,6-trifluorophenoxy)-3-benzyloxy-4-nitrobenzene

hydrogen

→

3-(3-hydroxy-4-amino-2,5,6-trifluorophenoxy)-6-aminophenol

용매

—

mixture

tetrahydrofuran

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONare added to the solution
2. 2
   기타is then hydrogenated at room temperature in an autoclave
3. 3
   기타the reaction is terminated
4. 4
   기타The yellow solution is evaporated to half in a rotary evaporator
5. 5
   workup.WAITan left
6. 6
   workup.WAITto stand at room temperature overnight, during which
7. 7
   기타the reaction product precipitates in crystalline form
8. 8
   기타The reaction product is then separated off
9. 9
   기타dried for 48 hours under nitrogen at, 40° C./10 mbar in a vacuum
10. 10
    기타drying cabinet

실험 절차

43.6 g of 1-(3-hydroxy-4-nitro-2,5,6-trifluorophenoxy)-3-benzyloxy-4-nitrobenzene prepared as described in Example 13 (0.1 mol) are dissolved in 400 ml of a mixture of tetrahydrofuran and ethyl acetate (volume ratio 1:1), and 4.4 g of Pd/C (palladium/carbon) are added to the solution. The mixture is then hydrogenated at room temperature in an autoclave with vigorous stirring using hydrogen at a pressure of 1 bar; after 3 days, the reaction is terminated. The yellow solution is evaporated to half in a rotary evaporator an left to stand at room temperature overnight, during which the reaction product precipitates in crystalline form. The reaction product is then separated off and dried for 48 hours under nitrogen at, 40° C./10 mbar in a vacuum drying cabinet.

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