Hydrochloric Acid → HCID 178484881, Verbindung

HRID 1835054

Reaktionsgleichung

Reaktionsgleichung von HRID 1835054
[CH3:1][C@H:2]([NH:10][CH3:11])[CH2:3][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[SH:12][C:13]1[N:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16].[CH3:22][C@H:23]([NH:31][CH3:32])[CH2:24][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1.[C:33]1([SH:44])[C:38]([Cl:39])=[C:37]([Cl:40])[C:36]([Cl:41])=[C:35]([Cl:42])[C:34]=1[Cl:43].C[C@H](NC)CC1C=CC=CC=1.Cl.Cl>C([O-])([O-])=O.[K+].[K+].[Ag].CCOCC.C(Cl)Cl.CO>[SH:12][C:13]1[N:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16].[CH3:1][C@H:2]([NH:10][CH3:11])[CH2:3][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[SH:12][C:13]1[N:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15]([OH:17])=[O:16].[CH3:22][C@H:23]([NH:31][CH3:32])[CH2:24][C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1.[C:33]1([SH:44])[C:34]([Cl:43])=[C:35]([Cl:42])[C:36]([Cl:41])=[C:37]([Cl:40])[C:38]=1[Cl:39]

Komponenten

12

Edukt 5

HCID 313Hydrochloric AcidHCID 8620Pentachlorothiophenol2×HCID 10836MethamphetamineHCID 66124(+)-Methamphetamine hydrochlorideHCID 178484881HCID 178484881, Verbindung

Produkt 2

HCID 178484881HCID 178484881, VerbindungHCID 178484882HCID 178484882, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 23954SilverKatalysatorHCID 887MethanolLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 11430Potassium CarbonateLösungsmittel

Versuchsvorschrift

Detection and Quantification of Methamphetamine using a Reactive Coating on Silver Foil: Silver foil was roughened and etched (Example 1d) followed by dip-coating in an methanol solution of MNA/methamphetamine containing 2 ppm of a CH2Cl2 solution of pentachlorothiolphenol (PCTP). The PCTP was used as an internal standard for quantification purposes. The coated foil surfaces were rinsed with ethanol to remove unbound MNA/methamphetamine and PCTP. The MNA/methamphetamine was synthesized by dissolving 186 mg methamphetamine hydrochloride in 15 mL of saturated aqueous K2CO3 to neutralize the hydrochloride. The freebase was then extracted from the aqueous solution using diethyl ether (Et2O). The ether was removed under reduced pressure and the methamphetamine re-dissolved in 8 mL of ethanol to which was added 169 mg 2-mercaptonicotinic acid (MNA) and 228 mg dicyclohexylcarbodiimide (DCC) in 2mL H2O. The reaction was gently refluxed under a nitrogen atmosphere for 2 hr. The MNA/methamphetamine reaction product was transferred to a separatory funnel using Et2O and extracted with additional Et2O followed by washes with saturated aqueous NaHCO3, H2O, and 10% HCI. Solvent was removed under reduced pressure. The product N-methyl-N-(1-methyl-2-phenylethyl)-2-mercaptopyridine-3-carboxamide (MNA/methamphetamine) was re-dissolved in methanol to form standard solutions in the concentration range of 0 ppm to 2500 ppm. SERS spectra were obtained from the MNA/methamphetamine/PCTP coated silver foil surfaces.

Aufarbeitung

  1. washThe coated foil surfaces were rinsed with ethanol
  2. customto remove unbound MNA/methamphetamine and PCTP
  3. extractionThe freebase was then extracted from the aqueous solution
  4. customThe ether was removed under reduced pressure
  5. dissolutionthe methamphetamine re-dissolved in 8 mL of ethanol to which
  6. additionwas added 169 mg 2-mercaptonicotinic acid (MNA) and 228 mg dicyclohexylcarbodiimide (DCC) in 2mL H2O
  7. temperatureThe reaction was gently refluxed under a nitrogen atmosphere for 2 hr
  8. customThe MNA/methamphetamine reaction product
  9. customwas transferred to a separatory funnel
  10. extractionextracted with additional Et2O
  11. customSolvent was removed under reduced pressure
  12. dissolutionThe product N-methyl-N-(1-methyl-2-phenylethyl)-2-mercaptopyridine-3-carboxamide (MNA/methamphetamine) was re-dissolved in methanol
  13. customto form standard solutions in the concentration range of 0 ppm to 2500 ppm

Quellen und Nachweise

ORD-Eintrag
ord-a8d72482e12a48198fbc2c08aabd52a5
Quelldatensatz
uspto-grants-2004_08
Patentnummer
US06770488B1

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