참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 3-(Methylsulfonyl)aniline hydrochloride | HCID 2735179 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Water methylene chloride | HCID 21908982 | — |
| 생성물 | 3-(Methylsulfonyl)phenol | HCID 637556 | 45.3% |
반응 단계
The title compound was prepared by a slightly modified literature procedure.* 3-aminophenyl methyl sulfone hydrochloride (1.18 g, 5.70 mmol) was suspended in water/CH2Cl2. The mixture was neutralized with 25% aqueous NaOH. The CH2Cl2 layer was isolated and evaporated to dryness. Aqueous H2SO4 (60%; 10 mL) was added to the residue and the solution was cooled to 0° C. A solution of NaNO2 (0.345 g, 5.00 mmol) in water (5 mL) was added dropwise. The solution was stirred at 0° C. for 30 min. and at 90° C. for 30 min. The reaction mixture was allowed to come to room temperature. Extraction with CH2Cl2, drying (MgSO4), and concentration gave 0.39 g (40%) of the title compound as a solid. MS m/z 172 (M)+. HRMS m/z calcd for C7H8O3S (M)+ 172.0194, found 172.0198.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06465467B1 |
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| 출처 데이터셋 | uspto-grants-2002_10 |
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| ORD ID | ord-b14b87f5bb384528ab0bafa84a3ffdc1 |
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| 출처 메모 | uspto-grants-2002_10 |
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