HRID1975603

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID11430

Potassium Carbonate

CK2O3

结构：COC(=O)C1=C(C)NC(C)=C(C(=O)OCCCl)C1c1cccc([N+](=O)[O-])c1

HCID3016888

2-Chloroethyl methyl 2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate

C18H19ClN2O6

HCID86747592

未命名化合物

PRODUCTS

生成物

结构：COC(=O)C1=C(C)NC(C)=C(C(=O)OCCON=Cc2ccc(Cc3ncc[nH]3)cc2)C1c1cccc([N+](=O)[O-])c1

HCID86747591

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

##STR36## 301 mg (0.763 mM) of 2-chloroethyl methyl 1,4-dihydro2,6-dimethyl-4-(3-nitrophenyl)pyridine-3,5-dicarboxylate and 155 mg (0.763 mM) of 4-(1-imidazolylmethyl)benzaldoxime were dissolved in 5 ml of dried acetonitrile, and then to the solution 58 mg (0.42 mM) of anhydrous potassium carbonate was added. After the mixture was heated under reflux for 15 hours, acetonitrile was distilled away and dichloromethane was added to the residue. After washing with water, the residue was dried over anhydrous sodium sulfate and dichloromethane was distilled away, and then the crystals were recrystallized from methanol, whereby the captioned compound was obtained. The yield was 400 mg (94%).

WORKUP

后处理

temperatureAfter the mixture was heated
temperatureunder reflux for 15 hours
distillationacetonitrile was distilled away
additiondichloromethane was added to the residue
washAfter washing with water
dry with materialthe residue was dried over anhydrous sodium sulfate and dichloromethane
distillationwas distilled away
customthe crystals were recrystallized from methanol, whereby the captioned compound
customwas obtained

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-e7e4464e74fa4aa0ba877773174fb7e0
来源数据集: uspto-grants-1994_02
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05286869
来源说明: uspto-grants-1994_02

反应 SMILES

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