反应详情

温度

50 °C

A one-gallon high-pressure reactor was charged with 4(2-methyl-2-nitropropyl)phenol (120 g, 614 mmol), HOAc (35.2 mL, 614 mmol), 5% Palladium on carbon (24 g) wetted with 2B3 EtOH (60 mL), and MeOH (1230 mL). The mixture was heated to 50° C. with agitation (600 rpm), and the reactor was purged with N2 and pressurized to 50 psi with H2. After 15.5 h the reactor was purged with N2, and the cooled mixture was filtered. The filter cake was washed with MeOH and the filtrate was concentrated to 514 g of slurry on a rotary evaporator. To this slurry was added EtOAc (2 L) with vigorous agitation. After stirring for 1 h, the resulting crystals were filtered and washed with a small amount of EtOAc. The product was dried overnight in a 45° C. vacuum oven to yield 118.83 g (86%) of product as small white needles (mp 211-216 ° C. dec). This material was 99% pure by HPLC analysis, and while another 9.00 g of material was obtained from the mother liquor it was found to be only 88 % pure.

1. customthe reactor was purged with N2
2. customAfter 15.5 h the reactor was purged with N2
3. filtrationthe cooled mixture was filtered
4. washThe filter cake was washed with MeOH
5. concentrationthe filtrate was concentrated to 514 g of slurry on a rotary evaporator
6. additionTo this slurry was added EtOAc (2 L) with vigorous agitation
7. filtrationthe resulting crystals were filtered
8. washwashed with a small amount of EtOAc
9. customThe product was dried overnight in a 45° C. vacuum oven