反应详情

61 g (0.26 mol) of 2,3-difluoro-4-(phenyldiazenyl)phenol from Example 3 and 1 g of Pd/C (10%) are initially charged in 800 ml of ethanol. The solution was degassed and aerated with hydrogen. The mixture was stirred at room temperature under a 1 bar hydrogen atmosphere for 18 hours. On completion of hydrogen uptake, the catalyst was filtered off and the filtrate was concentrated on a rotary evaporator, in the course of which the product already crystallized out. The resulting solid was filtered off, washed with a little cold ethanol and dried under high vacuum for 4 hours. 28 g (74%) of the desired compound were obtained as a light brown powder.

1. customThe solution was degassed
2. filtrationOn completion of hydrogen uptake, the catalyst was filtered off
3. concentrationthe filtrate was concentrated on a rotary evaporator, in the course of which the product
4. customalready crystallized out
5. filtrationThe resulting solid was filtered off
6. washwashed with a little cold ethanol
7. customdried under high vacuum for 4 hours