To a RBF which is in a cold water bath add 2.57 g of sodium borohydride, 40 mL of ethanol and 70 mL ethyl acetate with stirring, then add 4.07 g of β-nitro-3,4,5-trimethoxystyrene in small portions. Stir for 30 minutes after addition and add 50 mL of water, then as much of 50 % acetic acid is added until the gas evolution is ceased. The addition must be done very slowly. Then as much of sodium chloride is added until no more dissolves, the bottom aqueous layer is discarded. (Further mescaline may be recovered from the aqueous layer with ethyl acetate) The upper layer is then evaporated to dryness to obtain the crude product. The crude product is then recrystallized in ethanol.
Addition of β-nitro-3,4,5-trimethoxystyrene
Addition of water and acetic acid
The layers separating