6-(二甲氨基)-4,4-二苯庚烷-3-酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure of Example 5 is repeated using the methadone derivative 6-methylamino-4-phenyl-4-(4-hydroxyphenyl)heptan-3-one except for the following modifications. Instead of mixing the NaI125 reaction mixture on a Vortex mixer the mixture is shaken gently for 90 seconds and after addition of the bisulfite the mixture is shaken gently for 30 seconds. Finally 2.0 ml of 0.1 M Tris buffer pH 7.0 is used prior to the column chromatography step. The resulting above-captioned labeled antigen is obtained in Fractions #22-27 at a radioactive concentration of 10.5μCi/ml. EXAMPLE 7 Instead of mixing the NaI125 reaction mixture on a Vortex mixer the mixture is shaken gently for 30 seconds The resulting above-captioned labeled antigen is obtained in Fractions #22-27 at a radioactive concentration of 10.5μCi/ml

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure of Example 5 is repeated using the methadone derivative 6-methylamino-4-phenyl-4-(4-hydroxyphenyl)heptan-3-one except for the following modifications. Instead of mixing the NaI125 reaction mixture on a Vortex mixer the mixture is shaken gently for 90 seconds and after addition of the bisulfite the mixture is shaken gently for 30 seconds. Finally 2.0 ml of 0.1 M Tris buffer pH 7.0 is used prior to the column chromatography step. The resulting above-captioned labeled antigen is obtained in Fractions #22-27 at a radioactive concentration of 10.5μCi/ml. EXAMPLE 7 Instead of mixing the NaI125 reaction mixture on a Vortex mixer the mixture is shaken gently for 30 seconds The resulting above-captioned labeled antigen is obtained in Fractions #22-27 at a radioactive concentration of 10.5μCi/ml

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The procedure of Example 5 is repeated using the methadone derivative 6-methylamino-4-phenyl-4-(4-hydroxyphenyl)heptan-3-one except for the following modifications. Instead of mixing the NaI125 reaction mixture on a Vortex mixer the mixture is shaken gently for 90 seconds and after addition of the bisulfite the mixture is shaken gently for 30 seconds. Finally 2.0 ml of 0.1 M Tris buffer pH 7.0 is used prior to the column chromatography step. The resulting above-captioned labeled antigen is obtained in Fractions #22-27 at a radioactive concentration of 10.5μCi/ml. EXAMPLE 7 Instead of mixing the NaI125 reaction mixture on a Vortex mixer the mixture is shaken gently for 30 seconds The resulting above-captioned labeled antigen is obtained in Fractions #22-27 at a radioactive concentration of 10.5μCi/ml

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methadone (free base) was prepared for step B below by dissolving 10 grams of methadone hydrochloride in 100 mL of warm water at approximately 50° C. and crystallizing the free base out of solution by slowly adding 20 mL of a saturated aqueous potassium carbonate solution, pH 12.2 to the methadone hydrochloride solution with stirring. After crystallization was complete, the methadone crystals were filtered and redissolved in about 75 mL ethanol (ETOH). Following this the methadone was precipitated by the addition of 200 mL of water. The precipitate was filtered and dried in vacuo. The resulting yield of methadone was 8.79 g methadone or approximately 98%. crystallizing the free base out of solution by slowly adding 20 mL of a saturated aqueous potassium carbonate solution, pH 12.2 to the methadone hydrochloride solution After crystallization the methadone crystals were filtered redissolved in about 75 mL ethanol (ETOH) was precipitated by the addition of 200 mL of water The precipitate was filtered dried in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methadone (free base) was prepared for step B below by dissolving 10 grams of methadone hydrochloride in 100 mL of warm water at approximately 50° C. and crystallizing the free base out of solution by slowly adding 20 mL of a saturated aqueous potassium carbonate solution, pH 12.2 to the methadone hydrochloride solution with stirring. After crystallization was complete, the methadone crystals were filtered and redissolved in about 75 mL ethanol (ETOH). Following this the methadone was precipitated by the addition of 200 mL of water. The precipitate was filtered and dried in vacuo. The resulting yield of methadone was 8.79 g methadone or approximately 98%. crystallizing the free base out of solution by slowly adding 20 mL of a saturated aqueous potassium carbonate solution, pH 12.2 to the methadone hydrochloride solution After crystallization the methadone crystals were filtered redissolved in about 75 mL ethanol (ETOH) was precipitated by the addition of 200 mL of water The precipitate was filtered dried in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a 100 mL beaker equipped with a magnetic stir bar was charged methadone hydrochloride (3.0 g, 8.67 mmol) and water (30 g). Ammonium hydroxide (0.79 g, 22.6 mmol) was added to bring the pH to ˜9 (pH paper). The resulting solution was extracted with two 45 g portions of ethyl acetate and the combined organic layers were concentrated under reduced pressure at 40° C. The residue was dried under high vacuum to provide 2.2 g (82%) of a white solid which was analyzed by DSC (FIG. 1), FTIR (FIG. 2), PXRD (FIG. 3), and 1H-NMR (FIG. 4). The PXRD diffractogram was consisted with a crystalline product. To a 100 mL beaker equipped with a magnetic stir bar The resulting solution was extracted with two 45 g portions of ethyl acetate the combined organic layers were concentrated under reduced pressure at 40° C The residue was dried under high vacuum