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Methanol → HCID 178443526、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diethyl methylphosphonite | HCID 85063 | — |
| 反応物 | 1,4,5-Triphenyl-2-(7-bromoheptyloxy)imidazole | HCID 22916412 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178443526 | HCID 178443526 | 57.3% |
反応手順
A solution of 1,4,5-triphenyl-2-(7-bromoheptyloxy)-imidazole (1.75 g) and diethyl methylphosphonite (2.45 g) in toluene (10 ml) was heated at reflux temperature for 48 hours. Methanol and water were added and the mixture evaporated to an oil. This was chromatographed on silica gel (ethyl acetate/ethanol). The resulting oil slowly crystallised and was triturated with ether/petroleum ether, filtered then recrystallised from ethanol/ether to give ethyl 7-(1,4,5-triphenyl-imidazol-2-yloxy)heptane-methylphosphinate (1.06 g, 57%) as a white solid, m.p. 101°-2° C. Found: C, 72.05; H, 7.26; N, 5.52%; C31H37N2O3P; Requires: C, 72.07; H, 7.22; N, 5.42%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05648373 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-b4e6be7428ea45bfb31e2b127adfab45 |
| 出典メモ | uspto-grants-1997_07 |