関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Picric Acid | HCID 6954 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzyl chloromethyl ether | HCID 137983 | — |
| 反応物 | Bis-(4-chloro-phenyl)-(1H-imidazol-2-yl)-methanol | HCID 12433870 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-[(Benzyloxy)methyl]-alpha,alpha-bis(p-chlorophenyl)imidazole-2-methanol | HCID 3444069 | — |
反応手順
A mixture of 125 ml. of acetonitrile, 9.2 g of α,α-bis(p-chlorophenyl)imidazole-2-methanol (prepared according to Example III) and 1.5 g of sodium hydroxide was stirred for one hour. To the--now homogeneous--reaction mixture 500 mg of picric acid and a few crystals of potassium iodide were added and the mixture was heated to 50° C. A solution of 5.2 g of benzyloxymethyl chloride in 50 ml. of acetonitrile was then added dropwise and the reaction mixture was subsequently refluxed for 4 hours. The mixture was cooled and filtered and the filtrate was concentrated under reduced pressure. The residue was suspended in water and the suspension was extracted with diethyl ether. The extract was dried over sodium sulphate and the ether was distilled off. The solid residue obtained was crystallized from isopropyl alcohol. The product was then boiled four times with 75 ml. of petroleum ether (boiling range 60°-80° C.), the petroleum ether being decanted each time, after which it was once again crystallized from isopropyl alcohol. The substance was dried in vacuo for 10 hours at 110° C. 1-[(Benzyloxy)methyl]-α,α-bis(p-chlorophenyl)imidazole-2-methanol was obtained. Melting point 139°-141° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04152441 |
|---|
| 出典データセット | uspto-grants-1979_05 |
|---|
| ORD ID | ord-dfc1f11540a14a0b9581d3579560ae13 |
|---|
| 出典メモ | uspto-grants-1979_05 |
|---|