Can an experts out there please explain this method a little more? Is the 50%glycide ester similar to the pmk oil?
Method 9
Over a 4 hour period 23g of powdered sodium ethoxide is added to a stirred solution of 50g piperonal (40g benzaldehyde) and 61g bromoproprionate which is being chilled to below 0°C with a bath of ice and rock salt. After addition the solution is stirred for 12 hours at room temperature, then for an additional 6 hours at reflux. Ice water is added and the solution acidified with dilute acetic acid. The solution is extracted with ether, the ether washed with dilute sodium carbonate solution and dried through NazSO,. Distillation affords about 50% glycide ester intermediate (don't ask). 35g of this intermediate is refluxed for 5 hours in 150mL 10% NaOH in ethanol. The ethanol is then removed by distillation, 500mL dH.O is added to the residue and acidified with HCI, This acidified solution is extracted with ether and the ether layer separated. Remember, this is not an MDA or amphetamine we are talking about so acidifying is not going to bring this into the water. The ether is removed by simple distillation to give a residual oil. This oil remains alone in its flask and about 0.2g of copper powder is added. A condenser is placed on the flask and the oil is heated to 180°C for 18 hours. The procedure claims reflux occurs but Strike is doubtful that reflux as we know it will happen. After 18 hours the MD-P2P or P2P is vacuum distilled directly from the flask it just spent the last 18 hours in to give ~ 45% yield from the intermediate.
Method 9
Over a 4 hour period 23g of powdered sodium ethoxide is added to a stirred solution of 50g piperonal (40g benzaldehyde) and 61g bromoproprionate which is being chilled to below 0°C with a bath of ice and rock salt. After addition the solution is stirred for 12 hours at room temperature, then for an additional 6 hours at reflux. Ice water is added and the solution acidified with dilute acetic acid. The solution is extracted with ether, the ether washed with dilute sodium carbonate solution and dried through NazSO,. Distillation affords about 50% glycide ester intermediate (don't ask). 35g of this intermediate is refluxed for 5 hours in 150mL 10% NaOH in ethanol. The ethanol is then removed by distillation, 500mL dH.O is added to the residue and acidified with HCI, This acidified solution is extracted with ether and the ether layer separated. Remember, this is not an MDA or amphetamine we are talking about so acidifying is not going to bring this into the water. The ether is removed by simple distillation to give a residual oil. This oil remains alone in its flask and about 0.2g of copper powder is added. A condenser is placed on the flask and the oil is heated to 180°C for 18 hours. The procedure claims reflux occurs but Strike is doubtful that reflux as we know it will happen. After 18 hours the MD-P2P or P2P is vacuum distilled directly from the flask it just spent the last 18 hours in to give ~ 45% yield from the intermediate.
