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Sodium Phosphate, Dibasic → 4-Carbomethoxy-3-phthalimido-azetidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Phosphate, Dibasic | HCID 24203 | — |
| 反応物 | Potassium Persulfate | HCID 24412 | — |
| 反応物 | 4-Carbomethoxy-3-phthalimido-1-(p-methoxybenzyl)azetidin-2-one | HCID 23470178 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-Carbomethoxy-3-phthalimido-azetidin-2-one | HCID 23470061 | — |
反応手順
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°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04257947 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-af3051de722f49048d2c77dc82adbbf0 |
| 出典メモ | uspto-grants-1981_03 |