関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 3-Methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide | HCID 86735756 | — |
| 反応物 | HCID 178478652 | HCID 178478652 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178481663 | HCID 178481663 | 98.7% |
反応手順
175 g of anhydrous 3-methyl-2-(3-sulfopropylthio) benzothiazolium hydroxide was added to a mixture of 100 g of 5-aminobenzotriazole di-hydrochloride, 120 g of sodium acetate and 1000 ml of water under heating at 50° C with stirring in a 2000 ml flask. After stirring for 1 hour at 85° C the mixture was cooled (15° C) with water. The precipitate formed was collected by filtration, washed with water and then with acetonitrile to yield 135 g of crystals. These crystals were dissolved by heating (90° C) in 350 ml of dimethylformamide and the solution was treated with active carbon and filtered. By addition of 1400 ml of acetonitrile to the filtrate, crystals were formed. The crystals were collected to yield 121 g of the desired compound. The melting point was 240.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04095984 |
|---|
| 出典データセット | uspto-grants-1978_06 |
|---|
| ORD ID | ord-83e9387fa1c541aeaaebcb2cb3c4802e |
|---|
| 出典メモ | uspto-grants-1978_06 |
|---|