Method for synthesizing [<2>H3]-1-methylamino-2-phenylpropane
A technology of phenylpropane and synthetic method, which is applied in the field of forensic drug analysis, can solve the problems of harsh reaction conditions, time-consuming, time-consuming and cumbersome operations, etc., and achieve the effects of short reaction time, simple operation and short synthetic route
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Embodiment 1
[0034](1) 201 milligrams of phenylacetone and 150 milligrams of deuterated methylamine hydrochloride were added to 5 milliliters of methanol successively, and nitrogen protection was replaced. Under cooling in an ice bath, add 0.13 ml of tetraisopropyl titanate and 0.07 ml of triethylamine sequentially with a needle [need to activate phenylacetone with tetraalkyl titanate first, then add triethylamine to release deuteroformazine Amine, and finally deuterated methylamine and activated phenylacetone undergo addition reaction], start stirring. Monitor the reaction with GC / MS to generate the first intermediate (m / z43, 59, 91, 147), and stop the reaction after the phenylacetone (m / z 43, 92, 134) is completely consumed, and the reaction time is 5- 20 hours without post-treatment.
[0035] (2) Continue cooling with an ice bath, and add 90 mg of sodium borohydride in three batches under stirring. The reaction was monitored by GC / MS to produce [ 2 h 3 ]-1-methylamino-2-phenylpropan...
Embodiment 2
[0038] (1) 201 milligrams of phenylacetone and 150 milligrams of deuterated methylamine hydrochloride were added to 10 milliliters of ethanol successively, and nitrogen protection was replaced. Under cooling in an ice bath, add 0.15 ml of tetraethyl titanate and 0.10 ml of triethylamine sequentially with a needle [it is necessary to activate phenylacetone with tetraalkyl titanate first, and then add triethylamine to release deuterated methylamine. Finally, deuterated methylamine and the activated phenylacetone undergo an addition reaction] and start stirring. The reaction was monitored by GC / MS, and the first intermediate (m / z 43, 59, 91, 147) was generated. After the phenylacetone (m / z 43, 92, 134) was completely consumed, the reaction was stopped without post-treatment .
[0039] (2) Continue cooling with an ice bath, and add 100 mg of sodium borohydride in three batches under stirring. The reaction was monitored by GC / MS to produce [ 2 h 3 ]-1-methylamino-2-phenylpropan...
Embodiment 3
[0042] (1) 201 milligrams of phenylacetone, 225 milligrams of anhydrous sodium carbonate and 1.1 milliliters of 2mol / L deuterated methylamine methanol solution were added to 4 milliliters of methanol successively to replace the nitrogen protection. Under cooling in an ice bath, 0.15 ml of tetraisopropyl titanate was added with a needle, and stirring was started. The reaction was monitored by GC / MS, and the first intermediate (m / z 43, 59, 91, 147) was generated. After the phenylacetone (m / z 43, 92, 134) was completely consumed, the reaction was stopped without post-treatment.
[0043] (2) Continue cooling with an ice bath, and add 100 mg of potassium borohydride in three batches under stirring. The reaction was monitored by GC / MS to produce [ 2 h 3 ]-1-methylamino-2-phenylpropane (m / z 43,61,91), after the first reaction intermediate (m / z 43,59,91,147) is completely consumed, stop the reaction.
[0044] (3) Carefully add 4 ml of 2 mol / L ammonia solution to quench the reaction...
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