HRID1835053

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID1117

Sulfate

O4S-2

HCID3007

Amphetamine

C9H13N

HCID8620

Pentachlorothiophenol

C6HCl5S

2 次

HCID222898

未命名化合物

HCID178463689

未命名化合物

PRODUCTS

生成物

HCID178463689

未命名化合物

结构：CC(N)Cc1ccccc1.O=C(O)c1cccnc1S.Sc1c(Cl)c(Cl)c(Cl)c(Cl)c1Cl

HCID178463690

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

催化剂HCID23954

Silver

溶剂HCID6344

Dichloromethane

CH2Cl2

3 次

溶剂HCID11430

Potassium Carbonate

CK2O3

PROCEDURE

实验过程

Detection and Quantification of Amphetamine using a Reactive Coating on Silver Foil: Silver foil was roughened and etched (Example 1d) followed by dip-coating in an CH2Cl2 solution of MNA/amphetamine containing 3 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/amphetamine and PCTP. The MNA/amphetamine was synthesized by dissolving 363 mg amphetamine sulfate in 10 mL of an aqueous saturated solution of K2CO3 to neutralize the sulfate. The freebase drug was then extracted from the aqueous solution using CH2Cl2 followed by addition of 155 mg 2-mercaptonicotinic acid (MNA) and 206 mg dicyclohexylcarbodiimide (DCC). The reaction was gently refluxed overnight under a nitrogen atmosphere. The MNA/amphetamine reaction product was transferred to a separatory funnel with CH2Cl2 and washed with an aqueous saturated solution of NaHCO3 to neutralize unreacted MNA, followed by a wash with H2O and 10% HCI to neutralize unreacted freebase and DCC. Solvent was removed under reduced pressure. The product N-(1-methyl-2-phenylethyl)-2-mercaptopyridine-3-carboxamide (MNA/amphetamine) was re-dissolved in CH2Cl2 to form standard solutions in the concentration range of 0 ppm to 500 ppm. SERS spectra were obtained from the MNA/amphetamine/PCTP coated silver foil surfaces.

WORKUP

后处理

washThe coated foil surfaces were rinsed with ethanol
customto remove unbound MNA/amphetamine and PCTP
extractionThe freebase drug was then extracted from the aqueous solution
additionfollowed by addition of 155 mg 2-mercaptonicotinic acid (MNA) and 206 mg dicyclohexylcarbodiimide (DCC)
customThe MNA/amphetamine reaction product
washwashed with an aqueous saturated solution of NaHCO3
washa wash with H2O and 10% HCI
customSolvent was removed under reduced pressure
dissolutionThe product N-(1-methyl-2-phenylethyl)-2-mercaptopyridine-3-carboxamide (MNA/amphetamine) was re-dissolved in CH2Cl2
customto form standard solutions in the concentration range of 0 ppm to 500 ppm

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-4cb27c3c172f4fa58339fb44eca047fe
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

[NH2:1][CH:2]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH3:3].[SH:11][C:12]1[N:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15].[NH2:21][CH:22]([CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[CH3:23].[C:31]1([SH:42])[C:36]([Cl:37])=[C:35]([Cl:38])[C:34]([Cl:39])=[C:33]([Cl:40])[C:32]=1[Cl:41].S(O)(O)(=O)=O.NC(CC1C=CC=CC=1)C.S([O-])([O-])(=O)=O>C([O-])([O-])=O.[K+].[K+].[Ag].C(Cl)Cl>[SH:11][C:12]1[N:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15].[NH2:1][CH:2]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH3:3].[SH:11][C:12]1[N:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15].[NH2:21][CH:22]([CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[CH3:23].[C:31]1([SH:42])[C:32]([Cl:41])=[C:33]([Cl:40])[C:34]([Cl:39])=[C:35]([Cl:38])[C:36]=1[Cl:37]