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Potassium Iodide → 4-[Bis(4-fluorophenyl)hydroxymethyl]-N-phenyl-1-piperidinepropanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-chloro-N-phenylpropanamide | HCID 240404 | — |
| 反応物 | Bis(4-fluorophenyl)(piperidin-4-yl)methanol | HCID 11208889 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[Bis(4-fluorophenyl)hydroxymethyl]-N-phenyl-1-piperidinepropanamide | HCID 19992251 | 60.2% |
反応手順
A mixture of 2.0 g (0.007 mole) of α,α-bis(4-fluorophenyl)-4-piperidinemethanol, 2.6 g (0.014 mole) of 3-chloro-N-phenylpropanamide, 8.5 g (0.080 mole) of anhydrous sodium carbonate and 0.3 g (0.002 mole) of potassium iodide in 50 ml of N,N-dimethylformamide was heated on a steam bath for 16 hours. The mixture was poured into 500 ml of water and extracted twice with 250 ml portions of ethyl acetate. The combined extracts were washed with water and brine, dried (MgSO4) and concentrated under reduced pressure to give an off-white solid. The solid was recrystallized from methanol/2-propanol to yield 1.9 g (59%) of white solid, mp 190°-192° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05057524 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-b33e3e23225a46b285543c1fa7cb5240 |
| 出典メモ | uspto-grants-1991_10 |