関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | HCID 178526172 | HCID 178526172 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Modafinil acid | HCID 3085267 | — |
反応手順
A 50 L three-necked round bottom flask equipped with a mechanical stirrer, a 2 L dropping funnel, a nitrogen inlet and an internal temperature probe was charged with benzhydrylthioacetic acid (3.5 kg, 13.54 mol), methanol (14 L) and H2SO4 (72 g) solution in isopropyl alcohol (6.5 L). To this mixture was added 30% H2O2 solution in water (3.75 L) drop wise over 80 minutes maintaining the temperature below 30 degrees C. Reaction mixture was further stirred for 7 hours, which resulted in formation of a crystalline solid. The reaction was monitored using TLC and HPLC. The resulting solid was filtered and washed with water (4.0 L) to give benzhydrylsulfinylacetic acid (2.5 kg) as a colorless solid. The peroxide was quenched with a NaHSO3 solution.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07566805B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-314723f038fd407cace8ab487be6e5e8 |
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| 出典メモ | uspto-grants-2009_07 |
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