関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 4-(Methylthio)phenol | HCID 14086 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Methylsulfonyl)phenol | HCID 123350 | 30% |
| 生成物 | 4-(Methylsulfinyl)phenol | HCID 151936 | 42% |
反応手順
H2WO4 (0.029 g, 0.114 mmol) was stirred in H2O (10 ml). 50% NaOH (0.040 ml) was first added (pH>12) and then ACOH (0.040 ml) to reach pH 5. 4-methylsulfanyl-phenol (4 g, 0.029 mol) was added and the reaction mixture was heated to 65° C. 30% H2O2 in H2O (3 ml) was added in portions over 10 minutes. The reaction mixture was allowed to stir at room temperature for 1 h. 50% NaHSO3 was added to quench the reaction. Methylene chloride was added and the compound was washed with brine and purified by chromatography (0→10% EtOH in methylene chloride) to give 1.9 g of 4-methanesulfinyl-phenol (1) (42%) and 1.5 g of 4-methanesulfonyl-phenol (2) (30%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07915295B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-f5776f7b9372442dadd73c095ea2ab1e |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|
