Water → 2-(4,6-Dimethoxypyrimidine-2-yl)acetonitrile
Reaktionsgleichung
[C:1]([CH:3]([C:11]1[N:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[N:12]=1)C(OC(C)(C)C)=O)#[N:2].C1(C)C=CC=CC=1.CS(O)(=O)=O.O>C(OCC)(=O)C>[C:1]([CH2:3][C:11]1[N:12]=[C:13]([O:19][CH3:20])[CH:14]=[C:15]([O:17][CH3:18])[N:16]=1)#[N:2]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
Into a 50-ml eggplant-shaped flask provided with a magnetic stirrer and a reflux condenser were added 2.79 g (10 mmol) of tert-butyl 2-cyano-2-(4,6-dimethoxypyrimidin-2-yl)acetate, 10 ml of toluene and then 0.38 g (4 mmol) of methanesulfonic acid. The system inside was purged with nitrogen and stirred for 2 hours at 100° C. After the completion of a reaction, the system was cooled to room temperature; 30 ml water and 30 ml of ethyl acetate were added for phase separation; and re-extraction was conducted using 20 ml of ethyl acetate. Two ethyl acetate phases were combined, washed with saturated sodium chloride water, and dried over anhydrous sodium sulfate. Then, ethyl acetate was distilled off under reduced pressure to obtain 2-cyanomethyl-4,6-dimethoxypyrimidine as white crystal of 1.45 g. HPLC purity: 95.7% Yield: 81%
Aufarbeitung
- customInto a 50-ml eggplant-shaped flask provided with a magnetic stirrer and a reflux condenser
- customThe system inside was purged with nitrogen
- customAfter the completion of a reaction
- temperaturethe system was cooled to room temperature
- extractionand re-extraction
- washwashed with saturated sodium chloride water
- dry with materialdried over anhydrous sodium sulfate
- distillationThen, ethyl acetate was distilled off under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-15eeb50f2eed4a75bef0a3fed91f25b9
- Quelldatensatz
- uspto-grants-2014_06
- Patentnummer
- US08748605B2
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