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2-Nitrobenzyl alcohol → o-Nitrobenzyl benzylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Nitrobenzyl alcohol | HCID 11923 | — |
| 反応物 | Benzyl isocyanate | HCID 76639 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | o-Nitrobenzyl benzylcarbamate | HCID 54357994 | 67.9% |
反応手順
10 ml of toluene, 5.75 g of 2-nitrobenzyl alcohol and 5 g of benzyl isocyanate were heated to reflux for 3 hours in a nitrogen atmosphere. Following cooling of the mixture, 50 ml of toluene was added. This reaction solution was washed several times with water, and was then dehydrated with sodium sulfate. The sodium sulfate was then filtered out, and the solvent was removed from the filtrate by means of a rotary evaporator. The solid obtained was recrystallized from a hexane-toluene mixed solvent, producing 7.3 g of o-nitrobenzyl benzylcarbamate in the form of plate yellow crystals. This compound had a melting point of 110° to 111° C., and the infrared absorption spectrum was 3308 cm-1 : N--H, 1696 cm-1 : C=O, 1520 cm-1 : N--O.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05820944 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-3298aea7a9fa46d480cf89f625cec7f6 |
| 出典メモ | uspto-grants-1998_10 |