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Hydrochloric Acid → 5-Amino-1,3,4-thiadiazole-2-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetazolamide | HCID 1986 | — |
| 反応物 | Acetamide 2-acetylamino-1,3,4-thiadiazole-5-sulfonamide | HCID 67839732 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Amino-1,3,4-thiadiazole-2-sulfonamide | HCID 84724 | 85% |
反応手順
This is prepared by hydrolysis of the acetamide 2-acetylamino-1,3,4-thiadiazole-5-sulfonamide (acetazolamide). A slurry of 0.2 mol of acetazolamide in 600 mL of methanol is treated with 60 mL 12N HCl. This mixture is heated with stirring to reflux for 6 hours. Reaction progress is monitored using liquid chromatography. If reaction is not completed after 6 hours, another 30 mL of 12N HCl is added, and the mixture held at reflux for 2 hours. Methanol is then removed under reduced pressure. Product is recovered after raising the pH of the suspension to 7 by addition of NaOH at 0.4° , followed by filtration. Yield is between 85 and 98% of theoretical with 99% purity. KI =40 nM.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05242937 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-546e985c373d49ba8a1bca6b63eaccc9 |
| 出典メモ | uspto-grants-1993_09 |