MDMA/Synthesis: Difference between revisions

Line 40:

=== Chemicals and reagents ===

In the synthesis of MDMA, the following reagents were used: formic acid (98%), hydrochloric acid (36–38%), methylene chloride, sodium hydroxide, acetic acid (99.5%), acetone, diethyl ether, toluene, isopropanol, hydrogen peroxide ( 33%), sulfuric acid (95%) (all POCh, Poland, analytical grade), piperonal (99%, Aldrich, for synthesis), isosafrole (97%, Aldrich, for synthesis), safrole (97%, Aldrich, for synthesis), nitroethane (96%, Aldrich, for synthesis), cyclohexylamine (99%, Aldrich, for synthesis), ethyl formate (97%, Aldrich, for synthesis), hydrobromic acid (62%, Aldrich, analytical grade), methylamine solution (33% in abs. ethyl alcohol, Aldrich, analytical grade), methylamine aqueous solution (40%, Aldrich, analytical grade), diethyl ether (anhydrous, >99%, Aldrich, A.C.S. Reagent), methanol (Merck, HPLC grade), NaBH4 (Aldrich, for synthesis), NaBH3(CN) (Aldrich, for synthesis).

In the synthesis of MDMA, the following reagents were used:

* '''formic acid''' (98%)

* '''hydrochloric acid''' (36–38%)

* '''methylene chloride'''

* '''sodium hydroxide'''

* '''acetic acid''' (99.5%)

* '''acetone'''

* '''diethyl ether'''

* '''toluene'''

* '''isopropanol'''

* '''hydrogen peroxide''' (~33%)

* '''sulfuric acid''' (95%) (all POCh, Poland, analytical grade)

* '''piperonal''' (99%, Aldrich, for synthesis)

* '''isosafrole''' (97%, Aldrich, for synthesis)

* '''safrole''' (97%, Aldrich, for synthesis)

* '''nitroethane''' (96%, Aldrich, for synthesis)

* '''cyclohexylamine''' (99%, Aldrich, for synthesis)

* '''ethyl formate''' (97%, Aldrich, for synthesis)

* '''hydrobromic acid''' (62%, Aldrich, analytical grade)

* '''methylamine solution''' (33% in abs. ethyl alcohol, Aldrich, analytical grade)

* '''methylamine aqueous solution''' (40%, Aldrich, analytical grade)

* '''diethyl ether''' (anhydrous, >99%, Aldrich, A.C.S. Reagent)

* '''methanol''' (Merck, HPLC grade)

* '''NaBH4''' (Aldrich, for synthesis)

* '''NaBH3'''(CN) (Aldrich, for synthesis).

In impurity profiling experiments, the following reagents were used: carbonate buffer, pH 10 (10.7 ml, 0.1 M NaOH; 50 ml, 0.05 M NaHCO3; 39.3 ml H2O), ''n''-heptane (Aldrich, HPLC grade), phosphate buffer, pH 7 (Merck), diphenylamine (Supelco, used as internal standard).

In impurity profiling experiments, the following reagents were used:

* '''carbonate buffer''', pH 10 (10.7 ml, 0.1 M NaOH; 50 ml, 0.05 M NaHCO3; 39.3 ml H2O)

* '''''n''-heptane''' (Aldrich, HPLC grade)

* '''phosphate buffer''', pH 7 (Merck)

* '''diphenylamine''' (Supelco, used as internal standard).

=== Synthesis ===

@@ Line 40: / Line 40: @@
 === Chemicals and reagents ===
-In the synthesis of MDMA, the following reagents were used: formic acid (98%), hydrochloric acid (36–38%), methylene chloride, sodium hydroxide, acetic acid (99.5%), acetone, diethyl ether, toluene, isopropanol, hydrogen peroxide ( 33%), sulfuric acid (95%) (all POCh, Poland, analytical grade), piperonal (99%, Aldrich, for synthesis), isosafrole (97%, Aldrich, for synthesis), safrole (97%, Aldrich, for synthesis), nitroethane (96%, Aldrich, for synthesis), cyclohexylamine (99%, Aldrich, for synthesis), ethyl formate (97%, Aldrich, for synthesis), hydrobromic acid (62%, Aldrich, analytical grade), methylamine solution (33% in abs. ethyl alcohol, Aldrich, analytical grade), methylamine aqueous solution (40%, Aldrich, analytical grade), diethyl ether (anhydrous, >99%, Aldrich, A.C.S. Reagent), methanol (Merck, HPLC grade), NaBH<sub>4</sub> (Aldrich, for synthesis), NaBH<sub>3</sub>(CN) (Aldrich, for synthesis).
+In the synthesis of MDMA, the following reagents were used:
+* '''formic acid''' (98%)
+* '''hydrochloric acid''' (36–38%)
+* '''methylene chloride'''
+* '''sodium hydroxide'''
+* '''acetic acid''' (99.5%)
+* '''acetone'''
+* '''diethyl ether'''
+* '''toluene'''
+* '''isopropanol'''
+* '''hydrogen peroxide''' (~33%)
+* '''sulfuric acid''' (95%) (all POCh, Poland, analytical grade)
+* '''piperonal''' (99%, Aldrich, for synthesis)
+* '''isosafrole''' (97%, Aldrich, for synthesis)
+* '''safrole''' (97%, Aldrich, for synthesis)
+* '''nitroethane''' (96%, Aldrich, for synthesis)
+* '''cyclohexylamine''' (99%, Aldrich, for synthesis)
+* '''ethyl formate''' (97%, Aldrich, for synthesis)
+* '''hydrobromic acid''' (62%, Aldrich, analytical grade)
+* '''methylamine solution''' (33% in abs. ethyl alcohol, Aldrich, analytical grade)
+* '''methylamine aqueous solution''' (40%, Aldrich, analytical grade)
+* '''diethyl ether''' (anhydrous, >99%, Aldrich, A.C.S. Reagent)
+* '''methanol''' (Merck, HPLC grade)
+* '''NaBH<sub>4</sub>''' (Aldrich, for synthesis)
+* '''NaBH<sub>3</sub>'''(CN) (Aldrich, for synthesis).
-In impurity profiling experiments, the following reagents were used: carbonate buffer, pH 10 (10.7 ml, 0.1 M NaOH; 50 ml, 0.05 M NaHCO<sub>3</sub>; 39.3 ml H<sub>2</sub>O), ''n''-heptane (Aldrich, HPLC grade), phosphate buffer, pH 7 (Merck), diphenylamine (Supelco, used as internal standard).
+In impurity profiling experiments, the following reagents were used:
+* '''carbonate buffer''', pH 10 (10.7 ml, 0.1 M NaOH; 50 ml, 0.05 M NaHCO<sub>3</sub>; 39.3 ml H<sub>2</sub>O)
+* '''''n''-heptane''' (Aldrich, HPLC grade)
+* '''phosphate buffer''', pH 7 (Merck)
+* '''diphenylamine''' (Supelco, used as internal standard).
 === Synthesis ===