تفاعل #66363
ord-6d948e7e1edc4cd883fc2feba60835c2
معادلة التفاعل
الكواشف
المذيبات
ظروف التفاعل
درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىThe solvent was then removed under vacuum
- 2غسيلThe organic layer was washed with a saturated NaHCO3 solution (1×100 ml), brine (1×100 ml)
- 3تجفيفdried over Na2SO4
- 4أخرىThe filtrate was evaporated to dryness
الإجراء التجريبي
3,4-Dihydro-2H-pyran (10.83 g, 128.70 mmol) and p-toluenesulfonic acid (0.34 g, 1.75 mmol) were added to a solution of [(3-cyanophenyl-hydroxy-methyl]-phosphonic acid dimethyl ester (14.10 g, 58.50 mmol) in dry toluene (195 ml) and the reaction mixture was stirred under nitrogen atmosphere at 50° C. for 3 h. The solvent was then removed under vacuum and the residue was taken up with ethyl acetate (100 ml). The organic layer was washed with a saturated NaHCO3 solution (1×100 ml), brine (1×100 ml) and dried over Na2SO4. The filtrate was evaporated to dryness to give the crude [(3-cyano-phenyl)-(tetrahydro-pyran-2-yloxy)-methyl]phosphonic acid dimethyl ester as a yellow oil (19 g, 58.46 mmol, 100%).