Methanol → Methyl 4-chloro-3-(methoxycarbonylaminomethyl)benzoate
Reaktionsgleichung
Br[CH2:2][C:3]1[CH:4]=[C:5]([CH:10]=[CH:11][C:12]=1[Cl:13])[C:6]([O:8][CH3:9])=[O:7].[O-:14][C:15]#[N:16].[K+].CO.CN(C)[CH:22]=[O:23]>C(OCC)(=O)C.O>[Cl:13][C:12]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[CH2:2][NH:16][C:15]([O:23][CH3:22])=[O:14]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
16.0 g of the obtained methyl 3-bromomethyl-4-chlorobenzoate, 15.0 g of potassium cyanate and 35 ml of methanol were added to 200 ml of N,N-dimethylformamide, followed by stirring at 90° C. for 4 hours. After completion of the reaction, water was added to the reaction mixture, extraction with ethyl acetate was carried out, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude crystals were washed with isopropanol to obtain 25.2 g of methyl 4-chloro-3-(methoxycarbonylaminomethyl)benzoate as white crystals.
Aufarbeitung
- dry with materialthe organic layer was dried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe obtained crude crystals
- washwere washed with isopropanol
Quellen und Nachweise
- ORD-Eintrag
- ord-d4526409a12a456bb193fe73c51b7090
- Quelldatensatz
- uspto-grants-2004_11
- Patentnummer
- US06812229B1
Notizen zur Reaktion
Wird geladen…