Methanol → Methyl 1-(mercaptomethyl)cyclopropaneacetate
Reaktionsgleichung
C([S:4][CH2:5][C:6]1([CH2:9][C:10]#N)[CH2:8][CH2:7]1)(=O)C.[OH2:12].OS(O)(=O)=O.[CH3:18][OH:19]>>[SH:4][CH2:5][C:6]1([CH2:9][C:10]([O:19][CH3:18])=[O:12])[CH2:7][CH2:8]1Komponenten
5
Reaktionsbedingungen
- Temperatur
- 25 °C
Versuchsvorschrift
To a solution of the nitrile of Step 8 (45 g, 266 mmol) in MeOH (1.36 L) was added H2O (84 mL) and cone. H2SO4 (168 mL). The mixture was heated to reflux for 20 hours, cooled to 25° C., H2O (1 L) was added and the product was extracted with CH2Cl2 (2×1.5 L). The organic extract was washed with H2O and dried over Na2SO4. Concentration of the organic solution gave 36 g (93%) of the title compound.
Aufarbeitung
- temperatureThe mixture was heated
- temperatureto reflux for 20 hours
- extractionthe product was extracted with CH2Cl2 (2×1.5 L)
- extractionThe organic extract
- washwas washed with H2O
- dry with materialdried over Na2SO4
Quellen und Nachweise
- ORD-Eintrag
- ord-03e3a723725646409e1c008007a1794d
- Quelldatensatz
- uspto-grants-1995_08
- Patentnummer
- US05438141
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