تفاعل #215086
ord-af3051de722f49048d2c77dc82adbbf0
معادلة التفاعل
azetidinone
4-carbomethoxy-3-phthalimido-1-(p-methoxybenzyl)azetidin-2-one
potassium persulfate
disodium phosphate
→
4-carbomethoxy-3-phthalimido-azetidin-2-one
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe mixture was cooled
- 2أخرىthe acetonitrile removed in vacuum
- 3استخلاصthe aqueous residue saturated with sodium chloride and extracted
- 4درجة الحرارةwith warm (40°) hexane (3×100 ml)
- 5استخلاصThe ethyl acetate extract
- 6غسيلwas washed with sodium bicarbonate, brine
- 7أخرىdried
- 8أخرىevaporated to dryness
الإجراء التجريبي
A solution of 2.45 g (6.22 mmol) of the azetidinone in 250 ml of acetonitrile and 75 ml of water was degassed with argon. At 80°, a degassed solution of 23.5 g (87.2 mmol) of potassium persulfate and 7.77 g (55 mmol) of disodium phosphate was added in 6 portions over 1 hour. The mixture was cooled, the acetonitrile removed in vacuum, the aqueous residue saturated with sodium chloride and extracted with warm (40°) hexane (3×100 ml) then with ethyl acetate (5×125 ml). The ethyl acetate extract was washed with sodium bicarbonate, brine, dried and evaporated to dryness. Titration with ether gave 4-carbomethoxy-3-phthalimido-azetidin-2-one, m.p. 124°-6°.