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Triethylamine → 1,2,3-Thiadiazol-4-ylmethanol methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 1,2,3-Thiadiazol-4-ylmethanol | HCID 14727409 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,2,3-Thiadiazol-4-ylmethanol methanesulfonate | HCID 53789945 | 71.3% |
反応手順
A solution of 1,2,3-thiadiazol-4-ylmethanol (0.75 g, 6.5 mmol) in dichloromethane (20 mL) was cooled to 5° C. under a nitrogen atmosphere and treated with triethylamine (1.018 mL, 7.3 mmol) and methanesulfonyl chloride (0.565 mL, 7.3 mmol). After 15 min, the ice-bath was removed and the reaction mixture was stirred for 2 h. The solution was washed with 1N hydrochloric acid solution (2×2 mL) and water, dried (MgSO4 +MgO) and concentrated. The residue was purified by chromatography (silica gel column 1.5×21 cm) with ether as eluting solvent to give 0.90 g (71%) of 1,2,3-thiadiazol-4-ylmethanol methanesulfonate;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04732977 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-8499bae8663146e9bbdf2abc9c1fe95f |
| 出典メモ | uspto-grants-1988_03 |