Phosphorodithioate → Methyl 3-thiocarbamoylmethoxybenzoate

HRID 1602496

Reaktionsgleichung

Reaktionsgleichung von HRID 1602496
P([O-])([O-])([S-])=[S:2].[C:6]([CH2:8][O:9][C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=1)[C:13]([O:15][CH3:16])=[O:14])#[N:7]>C(OCC)(=O)C.Cl>[C:6]([CH2:8][O:9][C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=1)[C:13]([O:15][CH3:16])=[O:14])(=[S:2])[NH2:7]

Komponenten

4

Edukt 2

HCID 177047PhosphorodithioateHCID 14917017Methyl 3-(cyanomethoxy)benzoate

Produkt 1

HCID 19611422Methyl 3-thiocarbamoylmethoxybenzoateAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21866389Hydrogen chloride-ethyl acetateLösungsmittel

Versuchsvorschrift

4 N Hydrogen chloride-ethyl acetate solution (50 ml) and dithiophosphate=O,O-diethyl (4.47 ml, 26.67 mmol) were added in that order to methyl 3-cyanomethoxybenzoate (5.00 g, 26.15 mmol), and the resulting solution was stirred at room temperature for 12 hours. Crystals precipitated in the reaction solution were collected by filtration and washed with diethyl ether to give methyl 3-thiocarbamoylmethoxybenzoate (4.60 g, 78%).

Aufarbeitung

  1. customCrystals precipitated in the reaction solution
  2. filtrationwere collected by filtration
  3. washwashed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-443c714b642b44efbe4a71e33896aeaa
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05981559

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