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Guaifenesin → HCID 19762939、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Guaifenesin | HCID 3516 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 19762939 | HCID 19762939 | 60.1% |
反応手順
A solution of 3-(2-methoxy-phenoxy)-propane-1,2-diol (4.7 g) in pyridine, cooled at 5°-10° C., is treated under stirring with a solution of p-toluensulphonylchloride (4.5 g) in benzene (70 ml). The reaction mixture is stirred overnight at room temperature, then it is washed with 2N HCl (3×100 ml) and with water, dried on Na2SO4 and evaporated to dryness in vacuum. The oily residue is purified by column chromatography (silica gel 230-400 mesh hexane/AcOEt=3/1) to yield 5 g of 3-(2-methoxy-phenoxy)-2-hydroxy-1-propyl p-toluensulphonate (oil, NMR (--CDCl3):δ=2,4 3H (s) CH3SO2 ; δ=3,75-4,4 5H (m) OCH3 +OCH2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05212316 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-951d53943efa4613ae9d622148e68951 |
| 出典メモ | uspto-grants-1993_05 |