A further explanation of where my mind is going with this:
Chemicals needed:
Tannic acid
NaOH
Sulfuric acid + Methanol -? dimethyl sulfate
K2CO3
MgSO4 (or other dessicant)
Na2S2O3 (over the counter)
Bromine or Chlorine gas (easily made from their salts)
HCl
Acetic acid + Chlorine gas(MnO2+HCL)-?chloro acetic +NaOH ? sodium chloro acetate + NaNO2 ? Nitro methane + H2O
All OTC and cheap
Methyl 3,4,5-Trimethoxybenzoate: A solution of gallic acid hydrate (29.9 g) in DMF (100 ml) was added to a suspension of K2CO3 (97 g) in DMF (200 ml) with vigorous stirring. Dimethyl sulfate (66 ml) was added dropwise to the above mixture at 20-25°C. After completion of the addition, the mixture was stirred at room temperature for 2.5 h. The above procedure was repeated using a further amount of K2CO3 (44 g) and Me2SO4 (30 ml), then the reaction mixture was stirred at room temperature for a further 4.5 h, poured into water, and extracted with Et2O. The ethereal solution was dried over K2CO3 and evaporated to dryness. Recrystallization of the residue from MeOH gave pale yellow prisms (32.7 g), mp 85-86°C.
3,4,5-Trimethoxybenzyl Alcohol: A solution of Methyl 3,4,5-Trimethoxybenzoate (9.86 g) in abs. benzene (40 ml) was added dropwise to Vitride (22 ml) under ice cooling. After the mixture had been stirred at room temperature for a further hour the complex was decomposed with 25% H2SO4 (290ml). The benzene layer was separated from the aqueous layer, which was extracted with benzene. The organic layers were combined, washed with 5% NaHCO3 aq.. and then dried over MgSO4. Evaporation of the benzene solution gave an oily product (7.84 g).
3,4,5-Trimethoxybenzaldehyde
A solution of 39.6 g (0.2 mole) of 3,4,5-trimethoxybenzyl alcohol in 250 ml of methanol was stirred and cooled to 0°C. Bromine (54 ml) was added with stirring over a period of one hr keeping the temperature at 0°C. The stirred mixture was allowed to acquire room tempterature gradually and stirred further for 2 hr. A saturated solution of sodium thiosulfate (about 30 ml) was added to effect complete decomposition of excess bromine. 3,4,5-Trimethoxybenzaldehyde was filtered off and recrystallized from benzene to give 31 g (80%) as colourless needles, m.p. 73-74°C.
Reference: J. Chem. U.A.R., 11, No. 3, 401-404 (1968)
3) 3,4,5-Trimethoxy-nitrostyrene.
A solution of 40 cc of nitromethane and 100 g. of trimethoxybenzaldehyde in 200 cc alcohol is cooled to 0 deg C and while it is stirred mechanically there is introduced a solution of 45 g. pure potassium hydroxide in 45 cc water and 90 cc methanol at the rate of about one drop per second, care being taken that the temperature does not rise. Fifteen minutes after the addition is completed the solution is poured into 500 cc concentrated hydrochloric acid mixed with sufficient fee to assure its presence throughout the slow addition and to maintain the temperature of -10 deg C. The precipitated nitrostyrene is separated by filtration and washing and may be purified by recrystallizing from 700 cc alcohol. The pale yellow plates which melt at 120-121 deg C are obtained in a yield of approximately 78% of theory.
4) Mescaline.
[A] APPARATUS
A cell of porous porcelain (PC) (external dimensions 75x160 mm) with a glazed rim is placed in a glass jar of 500 cc capacity, surrounded by a cooling bath. The anode is a lead or carbon rod, surrounded by a glass coil; the cooling water flows through the coil and discharges into the cooling bath. The cathode is a sheet of lead (220x90x2 mm.), which previous to each experiment is electrolytically coated with lead peroxide, in a bath of dilute sulfuric acid.
REDUCTION
The cathode liquor consists of a solution of 30g. 3,4,5-trimethoxy- nitrostyrene in 100 cc glacial acetic acid and 100 cc alcohol, to which 50 cc conc. hydrochloric acid has been added. The anode compartment is filled, to the same level occupied by the catholyte, with a solution of 25 cc conc. sulfuric acid in 175 cc water.
The reduction requires 12 hours, using a current of 5-6 amperes; the cathode current density should be about 3 amperes per square centimeter. The temperature is regulated by the flow of the cooling water and the catholyte should be kept at 20 deg C for the first six hours; the temp is then allowed to rise until it reaches 40 deg C at the end of the reduction.
When the reduction is complete, the catholyte is filtered, evaporated in vacuum and the residue taken up in 300 cc water Unreduced nitrostyrene is extracted sucessively with ethyl acetate and with ether. The crude mescaline hydrochloride solution in a separatory funnel is then treated with a cold concentrated solution of 100 g. of sodium hydroxide and the liberated base exhaustively extracted with ether. The somewhat concentrated and dried (potassium carbonate) solution is treated with a stream of dry hydrogen chloride and the separated hydrochloride twice recrystallized from absolute alcohol. The pure mescaline hydrochloride, thus obtained in 77% yield, forms white leaflets melting at 184°C.
For OTC Nitromethane I was thinking:
Chloroacetic acid is prepared industrially via two routes. The predominant method involve chlorination of acetic acid:
CH3CO2H + Cl2 ? ClCH2CO2H + HCl
The reaction of sodium chloroacetate with sodium nitrite in aqueous solution produces this compound:[2]
ClCH2COONa + NaNO2 + H2O ? CH3NO2 + NaCl + NaHCO3
*upon looking at this more I realized that a rough reducing agent is necessary to reduce the ester. I am working on an electrolytic research project for university and am hoping this will cut out the need for LAH for reduction.
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