関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 3-(Chlorosulfonyl)-4-methoxybenzoic acid | HCID 3854888 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 3-(5-Carboxy-2-methoxy-phenyldisulfanyl)-4-methoxy-benzoic acid | HCID 12425751 | 99.7% |
反応手順
45 g (179.5 mmol) of 3-chlorosulfonyl-4-methoxy-benzoic acid were suspended in 200 ml of acetic acid and warmed to 40° C. Then a solution of 85.1 g (448.8 mmol) tin(II) chloride in 100 ml of hydrochloric acid was added within 15 min and the mixture was stirred for 2 h under reflux. The hot solution was added dropwise to 2000 ml of ice/water. The formed precipitate was collected by suction, washed with water and dried. 32.8 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08362073B2 |
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| 出典データセット | uspto-grants-2013_01 |
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| ORD ID | ord-34cb0a93d7814fd0a5881c323654ccc9 |
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| 出典メモ | uspto-grants-2013_01 |
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