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All 4 posts Subject: Some more reference Please login to post Down

murmur
(HyperLab Bee)
06-02-03 09:13
No 437170
      Some more reference

Journal of Chemical Research (S) 1981, 192
Dibenzo-18-crown-6 as phase transfer catalyst in Bockmuhl's synthesis of methadone
http://hyperlab.bravepages.com/JChemRes1981%28S%29.djvu
I could't get the Miniprit version of this artcle because in a library this volume is not available.

Rhodium
(Chief Bee)
06-02-03 14:18
No 437232
User Picture       Miniprint

Edit: The full Miniprint edition has been posted in Post 481630 (Aurelius: "PTC Synthesis of Methadone", Methods Discourse)

murmur
(HyperLab Bee)
06-04-03 10:32
No 437755
      Deuterated Methadone
(Rated as: excellent)

Synthesis and Physico-Chemical Properties of (RS)-6-bis(Trideuteriomethyl)amino-4,4-Diphenylheptan-3-one Hydrochloride (Methadone-d₆)
B.M. Gérardy, et. al.
J. Lab. Comp. Radiopharm. 22(1), 5-22 (1985) (https://www.rhodium.ws/djvu/methadone-d6.djvu)

Experimental section

(R,S)-2,2-diphenyl-4-ditrideuteromethylaminopentanenitrile (1)
To a solution of 6 g (68.5 mmol) of ditrideuteromethylamine hydrochloride dissolved in 3 ml of water was added 2.8 g (70 mmol) of NaOH disolved in 5 ml H₂O. Under stirring, a filtered solution of the above mixture was added over 1 h period to 4.77 g (82.2 mmol) of freshly redistilled propylene oxide. After 12 hrs at RT, 90 ml of benzene were added and the reaction mixture was fractionnally distilled. The fractions under 81 °C and above 99°C were discarded. The remaining 4.07 g consisting of a mixture of isomeric aminoalcohols (1-ditrideutromethylamino-2-propanol and 2-ditrideutromethylamino-1-propanol)were dissolved in 25 ml of dry CHCl₃(ethanol free) and treated by 14.4 g (113 mmol) of freshly redistilled thionyl chloride. The reaction mixture was stirred and heated at 55°C for 2 hrs. After evaporating the solvent under reduced pressure, a residue weighing 5.42 g consisting of a mixture of isomeric beta-chloroamines was obtained. Then, to a solution of 6 g (31 mmol)of diphenylacetonitrile and 0.2 g of dibenzo-18-crown-6 in 6 ml DMSO were added under stirring 5 g (125 mmol) of NaOH in 5 ml of distilled H₂O in one portion and 5.42 g of beta-chloroamines over one hour period. The reaction mixture was gradually heated up to 70 °C and this temperature was maintained for 3 h. After cooling, the basis fraction was isolated in the usual way and recrystallysed from n-hexane and then from n-heptane to yield 2.8 g (32.5%) of (1), mp=81-82°C. This material was pure in GLC.

(R,S)-4,4-diphenyl-6-ditrideuteromethylaminoheptan-3-one hydrochloride (2)
This material was synthesed according to the procedure described by Bockmuhl and Ehrhardt (J.Liebigs Ann.Chem 561(1949)52, Post 483448 (Rhodium: "Bockmühl's Original Methadone Synthesis", Methods Discourse)). To a suspension of 0.24 g (10 mmol) of Mg in 5 ml of dry ether was added 2.55 g (23 mmol) of ethyl bromide. After of completition of the reaction, a solution of 2.8 g (9.86 mmol) of(1) in 3 ml of dry xylene was added to the reaction mixture under stirring. The ether was distilled off in dry conditions; the reaction mixture was heated under reflux for 1 h and then decomposed with 100 ml of 8 N HCl. After the usual work up, 2.48 g (79%) of (2) were obtained. The hydrochloride crystallized from ethanolic HCl was obtained in 72% yield. It was recrystallized from IPA to constant melting point (mp=233°C) This product was pure in GLC and HPTLC.

murmur
(HyperLab Bee)
06-09-03 09:19
No 438801
      Tritiated Methadone
(Rated as: good read)

Preparation of Methadone and Some Congeners Labeled with Tritium in the Aromatic Rings
J.A. Kepler, et. al.
J. Lab. Comp. Radiopharm. 19(2), 271-282 (1982) (https://www.rhodium.ws/djvu/methadone-tritium.djvu)

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	All 4 posts		Subject: Some more reference		Please login to post		Down


		murmur (HyperLab Bee) 06-02-03 09:13 No 437170				Some more reference
						Journal of Chemical Research (S) 1981, 192 Dibenzo-18-crown-6 as phase transfer catalyst in Bockmuhl's synthesis of methadone http://hyperlab.bravepages.com/JChemRes1981%28S%29.djvu I could't get the Miniprit version of this artcle because in a library this volume is not available.



		Rhodium (Chief Bee) 06-02-03 14:18 No 437232				Miniprint
						Edit: The full Miniprint edition has been posted in Post 481630 (Aurelius: "PTC Synthesis of Methadone", Methods Discourse)



		murmur (HyperLab Bee) 06-04-03 10:32 No 437755				Deuterated Methadone (Rated as: excellent)
						*Synthesis and Physico-Chemical Properties of (RS)-6-bis(Trideuteriomethyl)amino-4,4-Diphenylheptan-3-one Hydrochloride (Methadone-d₆)* B.M. Gérardy, et. al. J. Lab. Comp. Radiopharm. 22(1), 5-22 (1985) (https://www.rhodium.ws/djvu/methadone-d6.djvu) Experimental section (R,S)-2,2-diphenyl-4-ditrideuteromethylaminopentanenitrile (1) To a solution of 6 g (68.5 mmol) of ditrideuteromethylamine hydrochloride dissolved in 3 ml of water was added 2.8 g (70 mmol) of NaOH disolved in 5 ml H₂O. Under stirring, a filtered solution of the above mixture was added over 1 h period to 4.77 g (82.2 mmol) of freshly redistilled propylene oxide. After 12 hrs at RT, 90 ml of benzene were added and the reaction mixture was fractionnally distilled. The fractions under 81 °C and above 99°C were discarded. The remaining 4.07 g consisting of a mixture of isomeric aminoalcohols (1-ditrideutromethylamino-2-propanol and 2-ditrideutromethylamino-1-propanol)were dissolved in 25 ml of dry CHCl₃(ethanol free) and treated by 14.4 g (113 mmol) of freshly redistilled thionyl chloride. The reaction mixture was stirred and heated at 55°C for 2 hrs. After evaporating the solvent under reduced pressure, a residue weighing 5.42 g consisting of a mixture of isomeric beta-chloroamines was obtained. Then, to a solution of 6 g (31 mmol)of diphenylacetonitrile and 0.2 g of dibenzo-18-crown-6 in 6 ml DMSO were added under stirring 5 g (125 mmol) of NaOH in 5 ml of distilled H₂O in one portion and 5.42 g of beta-chloroamines over one hour period. The reaction mixture was gradually heated up to 70 °C and this temperature was maintained for 3 h. After cooling, the basis fraction was isolated in the usual way and recrystallysed from n-hexane and then from n-heptane to yield 2.8 g (32.5%) of (1), mp=81-82°C. This material was pure in GLC. (R,S)-4,4-diphenyl-6-ditrideuteromethylaminoheptan-3-one hydrochloride (2) This material was synthesed according to the procedure described by Bockmuhl and Ehrhardt (J.Liebigs Ann.Chem 561(1949)52, Post 483448 (Rhodium: "Bockmühl's Original Methadone Synthesis", Methods Discourse)). To a suspension of 0.24 g (10 mmol) of Mg in 5 ml of dry ether was added 2.55 g (23 mmol) of ethyl bromide. After of completition of the reaction, a solution of 2.8 g (9.86 mmol) of(1) in 3 ml of dry xylene was added to the reaction mixture under stirring. The ether was distilled off in dry conditions; the reaction mixture was heated under reflux for 1 h and then decomposed with 100 ml of 8 N HCl. After the usual work up, 2.48 g (79%) of (2) were obtained. The hydrochloride crystallized from ethanolic HCl was obtained in 72% yield. It was recrystallized from IPA to constant melting point (mp=233°C) This product was pure in GLC and HPTLC.



		murmur (HyperLab Bee) 06-09-03 09:19 No 438801				Tritiated Methadone (Rated as: good read)
						Preparation of Methadone and Some Congeners Labeled with Tritium in the Aromatic Rings J.A. Kepler, et. al. J. Lab. Comp. Radiopharm. 19(2), 271-282 (1982) (https://www.rhodium.ws/djvu/methadone-tritium.djvu)

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