Reaktion #6434

Reaktionsgleichung

methanol

diethyl 3-hydroxy-3-methyl-3-(1-methyl-1,2,4-triazol-5-yl)propylphosphonate

TMSBr

propylene oxide

→

3-hydroxy-3-methyl-3-(1-methyl-1,2,4-triazol-5-yl)propyl-phosphonic acid

Lösungsmittel

CH2Cl2

diethylether

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter stirring for 2 hours
2. 2
   Sonstigegave colourless
3. 3
   Sonstigeprecipitates which
4. 4
   Sonstigewere collected on a glass
5. 5
   Filtrationfilter under nitrogen
6. 6
   Waschenwashed with diethylether
7. 7
   Sonstigedried in vacuo

Vorschrift

To a solution of diethyl 3-hydroxy-3-methyl-3-(1-methyl-1,2,4-triazol-5-yl)propylphosphonate (1.2 g, 4.12 mmol) in CH2Cl2 (24 ml) was added TMSBr (2.72 ml, 20.6 mmol, 5 eq) at room temperature under nitrogen. The reaction mixture was stirred for 16 hours. Then methanol (12 ml) was added to the mixture. After stirring for 2 hours, addition of propylene oxide (2.4 ml) and dilution with diethylether gave colourless precipitates which were collected on a glass filter under nitrogen, washed with diethylether, and dried in vacuo to give pure 3-hydroxy-3-methyl-3-(1-methyl-1,2,4-triazol-5-yl)propyl-phosphonic acid, compound no 5.001 (0,63 g, 65% yield). ##STR49##

Quelle