4-MeO-PCP (methoxydine), as of 25 June 2023, is not a controlled substance in the USA.
It can be made in a similar way as PCP.
STEP 1: Preparing the intermediate
6.3g of sodium bisulfite in 21mL of water was cooled in an ice bath. 5.3g (5.03 mL) of cyclohexanone was added with rapid stirring, which results in a thick white slurry. A solution of 3.93g of potassium cyanide in 8.17mL piperidine is added to the slurry, which turns into a 2-phase reaction mixture. Allow to stir overnight.
The next morning, stop stirring and cool on ice. Upper oily phase soon crystallized into ice-like crystals. Removed via filtration, washed with cool water, and dried between paper towels..
Step 2: Preparing the Grignard
1.9g of Mg turnings were placed in a RBF, along with a stirbar and 30mL of dry ether. In a second flask, a solution of 4-MeO-Bromobenzene (also known as 4-bromo-anisole) in 10mL ether was prepared. Approx. 9mL of
the bromobenzene soln was added to the flask containing ether/Mg.
This flask was gently heated and stirred until rxn began, as indicated by a cloudy gray precipitate forming. The remaining ether/bromobenzene soln. was added at a rate that allowed for gentle reflux.
NOTE: This must be done in dry conditions. All glassware was dried in an oven at 350F for 1 hour.
Step 3: Reaction between PCC and the Grignard
A solution of 3.5g of the compound prepared in step 1 was dissolved in approx. 10mL of toluene. This solution was dried over calcium chloride, filtered, then diluted with an equal amount of ether. This was slowly added to the Grignard prepared in step 2, followed by heating and stirring for 2 hours.
The reaction mixture was poured onto a mix of several grams of ammonium chloride and ice, with stirring. After bubbling stopped, several grams of NaOH was added, and mixture shaken in a sep funnel. Lower aquoeus phase was seperated, shaken with fresh ether and discarded.
The combined organic phases washed 3x with water, water layers discarded. Organic layer was extracted 3 times with dilute HCl. Acid layers were basified with NaOH and extracted with ether. Combined layers were evaporated to give 2.5g of colorless oil. After sitting for 2 days, cooling in the freezer, oil crystallized into colorless crystals.
It can be made in a similar way as PCP.
STEP 1: Preparing the intermediate
6.3g of sodium bisulfite in 21mL of water was cooled in an ice bath. 5.3g (5.03 mL) of cyclohexanone was added with rapid stirring, which results in a thick white slurry. A solution of 3.93g of potassium cyanide in 8.17mL piperidine is added to the slurry, which turns into a 2-phase reaction mixture. Allow to stir overnight.
The next morning, stop stirring and cool on ice. Upper oily phase soon crystallized into ice-like crystals. Removed via filtration, washed with cool water, and dried between paper towels..
Step 2: Preparing the Grignard
1.9g of Mg turnings were placed in a RBF, along with a stirbar and 30mL of dry ether. In a second flask, a solution of 4-MeO-Bromobenzene (also known as 4-bromo-anisole) in 10mL ether was prepared. Approx. 9mL of
the bromobenzene soln was added to the flask containing ether/Mg.
This flask was gently heated and stirred until rxn began, as indicated by a cloudy gray precipitate forming. The remaining ether/bromobenzene soln. was added at a rate that allowed for gentle reflux.
NOTE: This must be done in dry conditions. All glassware was dried in an oven at 350F for 1 hour.
Step 3: Reaction between PCC and the Grignard
A solution of 3.5g of the compound prepared in step 1 was dissolved in approx. 10mL of toluene. This solution was dried over calcium chloride, filtered, then diluted with an equal amount of ether. This was slowly added to the Grignard prepared in step 2, followed by heating and stirring for 2 hours.
The reaction mixture was poured onto a mix of several grams of ammonium chloride and ice, with stirring. After bubbling stopped, several grams of NaOH was added, and mixture shaken in a sep funnel. Lower aquoeus phase was seperated, shaken with fresh ether and discarded.
The combined organic phases washed 3x with water, water layers discarded. Organic layer was extracted 3 times with dilute HCl. Acid layers were basified with NaOH and extracted with ether. Combined layers were evaporated to give 2.5g of colorless oil. After sitting for 2 days, cooling in the freezer, oil crystallized into colorless crystals.
