HRID1835054

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID313

Hydrochloric Acid

ClH

HCID8620

Pentachlorobenzenethiol

C6HCl5S

2 次

HCID10836

Methamphetamine

C10H15N

HCID66124

S-(+)-Methamphetamine hydrochloride

C10H16ClN

HCID178484881

未命名化合物

PRODUCTS

生成物

HCID178484881

未命名化合物

结构：CN[C@@H](C)Cc1ccccc1.O=C(O)c1cccnc1S.Sc1c(Cl)c(Cl)c(Cl)c(Cl)c1Cl

HCID178484882

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

催化剂HCID23954

Silver

溶剂HCID887

Methanol

CH4O

溶剂HCID3283

Diethyl Ether

C4H10O

溶剂HCID6344

Dichloromethane

CH2Cl2

溶剂HCID11430

Potassium Carbonate

CK2O3

PROCEDURE

实验过程

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.

WORKUP

后处理

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

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-a8d72482e12a48198fbc2c08aabd52a5
来源数据集: uspto-grants-2004_08
DOI: 10.6084/m9.figshare.5104873.v1
专利: US06770488B1
来源说明: uspto-grants-2004_08

反应 SMILES

[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]