Dimethylformamide → propargyl N-methoxy-2,4-dichlorobenzimidate

HRID 3405

Reaktionsgleichung

Reaktionsgleichung von HRID 3405
[CH3:1][O:2][NH:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12].C(=O)([O-])[O-].[K+].[K+].[CH2:20](Br)[C:21]#[CH:22].CN(C)C=O>O>[CH3:1][O:2][N:3]=[C:4]([O:13][CH2:22][C:21]#[CH:20])[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12]

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 189350352,4-dichloro-N-methoxybenzamide

Produkt 1

HCID 53654798propargyl N-methoxy-2,4-dichlorobenzimidateAusbeute 29,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

1.0 g of N-methoxy-2,4-dichlorobenzamide, 0.75 g of potassium carbonate and 0.65 g of propargyl bromide were added to 10 ml of N,N-dimethylformamide, and the mixture was stirred for 3 hours. After completion of the reaction, water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried, concentrated and purified by silica gel column chromatography to obtain 0.35 g of propargyl N-methoxy-2,4-dichlorobenzimidate.

Aufarbeitung

  1. additionwas added to the reaction solution
  2. extractionthe mixture was extracted with ethyl acetate
  3. customThe extract was dried
  4. concentrationconcentrated
  5. custompurified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-bc47ddbc82764811b755545cf676a4fc
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05733935

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