I have a lot of articles about the Fe/HCl reduction of phenyl-2-nitropropene to the oxime and the subsequent hydrolysis. However, in my eyes,
Patent US2557051
gives the most convenient procedure.
Example 1200 grams of o-methoxybenzaldehyde, 150 grams of nitroethane and 40 mL of n-butylamine were dissolved in 400 mL of toluene in a flask equipped with a reflux condenser and a suitable water seperation trap and the mixture heated under reflux until the collection of water ceased.
The water trap was removed from the system and a stirrer introduced into the flask. 750 grams of finely-divided iron, 1500 mL of water and 7 grams of ferric chloride were then added. The mixture was then heated to boiling and, while stirring vigorously, 750 mL of concentrated HCl was added dropwise over a period of 4 hours. The reaction mixture was subjected to steam distillation, 18 liters of distillate being collected. The toluene layer was removed and the aqueous layer was extracted with fresh toluene. The combined toluene extracts were fractionally distilled, yielding 247 grams of o-methoxyphenylacetone boiling at 126-132 °C / 14 mm Hg. Yield: 75.5 %
Example 3In the same manner as given for Example 3, approximately equimolar proportions of benzaldehyde and nitroethane are condensed in toluene in the presence of n-butylamine at about reflux temperature, the distillate collected, water removed, and the toluene removed to the reaction zone. After about 6 hours the calculated quantity of water has been removed from the reaction zone and iron, water and ferric chloride are added thereto. Concentrated HCl is then adde dropwise to the mixture at about reflux temperature with vigorous agitation over a period of 6 hours. Upon steam distillation of the product and the removal of the toluene, extraction of the aqueous layer with fresh toluene, and fractional distillation of the extracts, approximately 75 percent of the theoretical yield of desired phenylactone is obtained.
IMHO, this is THE method for the preparation of P2P.
The next step will be something like:
P2P + MeNH2 --> meth
I suggest a Parr hydrogenation with PtO2 as catalyst.