関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Benzenesulfinic acid | HCID 12057 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | Benzenesulfinic acid, sodium salt | HCID 2723840 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzenesulfonyl-1,2-dicarbisopropoxy hydrazine | HCID 20385926 | — |
反応手順
To one-half mole of sodium benzenesulfinate in water in a 2 liter beaker is introduced 49 g (0.5 mole) of concentrated sulfuric acid. To the resulting suspension of benzenesulfinic acid is then added 101 g (0.5 mole) of diisopropyl azodicarboxylate. The mixture is stirred and heated to 60° C. (30 minutes). The yellow color of the azo ester gradually disappears. The oily product is extracted with benzene and separated from the lower aqueous layer. Removal of the benzene by evaporation leaves a clear oil which crystallizes when introduced into an 80/20 hexane/benzene mixture. The filtered crystals are dried at 60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04175200 |
|---|
| 出典データセット | uspto-grants-1979_11 |
|---|
| ORD ID | ord-58cd4acef3d14a2cb43d04d5449aeec1 |
|---|
| 出典メモ | uspto-grants-1979_11 |
|---|
