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Oxalic Acid → 5-[2-[4[Bis(4-fluorophenyl)hydroxymethyl]-1-piperidinyl]ethyl]-3-methyl-2-oxazolidinone oxalate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Bis(4-fluorophenyl)(piperidin-4-yl)methanol | HCID 11208889 | — |
| 反応物 | 5-(2-Chloro-ethyl)-3-methyl-oxazolidin-2-one | HCID 14698746 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 5-[2-[4[Bis(4-fluorophenyl)hydroxymethyl]-1-piperidinyl]ethyl]-3-methyl-2-oxazolidinone oxalate | HCID 19836722 | 71% |
反応手順
A mixture of 3.0 g (0.01 mole) of α,α-bis(p-fluorophenyl)-4-piperidinemethanol, 1.6 g (0.01 mole) of 5-(2-chloroethyl)-3-methyl-2-oxazolidinone, 5.3 g (0.085 mole) of anhydrous sodium carbonate and 0.3 g of potassium iodide in 100 ml of 1-butanol was heated at reflux for 20 hr. The mixture was concentrated under reduced pressure and the residue was partitioned between water and benzene. The benzene layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give a gum as residue. The gum was converted to the oxalic acid salt, recrystallizing from absolute ethanol to give 3.7 g (71%) of white powder, m.p. 124°-134° C. with decomposition.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04886794 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-e650102e8b3d4db68039db5dbc670305 |
| 出典メモ | uspto-grants-1989_12 |