Reaktionsgleichung
[CH:1]1([CH2:4][O:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[O:12][CH2:13][CH2:14][OH:15])[CH2:3][CH2:2]1.C(N(CC)CC)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25].O>C(Cl)Cl>[CH3:23][S:24]([O:15][CH2:14][CH2:13][O:12][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[O:5][CH2:4][CH:1]1[CH2:2][CH2:3]1)(=[O:26])=[O:25]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
2-Cyclopropylmethyloxy-1-(2-hydroxyethyloxy)benzene (2.7 g, 13.0 mmol), prepared as in Example 1, Step (a), and triethylamine (2.7 mL, 19.5 mmol) were dissolved in methylene chloride (20 mL) and the solution was cooled in an ice bath. Methanesulfonyl chloride (1.2 mL, 15.5 mmol) in methylene chloride (10 mL) was added dropwise to the solution and the mixture was stirred at 0° C. for 30 minutes. Water was added and the mixture was stirred vigorously at room temperature for 15 minutes. The mixture was extracted into methylene chloride. The organic phase was separated, washed with 2N hydrochloric acid and then brine, and dried over magnesium sulfate. Evaporation gave 2-[2-(cyclopropylmethyloxy)phenoxy]ethyl methanesulfonate (3.7 g, 12.9 mmol) as a white solid, m.p. 90°-91° C.
Aufarbeitung
- temperaturethe solution was cooled in an ice bath
- stirringthe mixture was stirred vigorously at room temperature for 15 minutes
- extractionThe mixture was extracted into methylene chloride
- customThe organic phase was separated
- washwashed with 2N hydrochloric acid
- dry with materialbrine, and dried over magnesium sulfate
- customEvaporation
Quellen und Nachweise
- ORD-Eintrag
- ord-41b83493471243339b47beefd2585755
- Quelldatensatz
- uspto-grants-1995_07
- Patentnummer
- US05436264
Verknüpfte Notizen
Wird geladen…