関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methyl 2-(3-mercaptophenyl)acetate | HCID 14820216 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Methyl [3-(chlorosulfonyl)phenyl]acetate | HCID 23388821 | 79% |
反応手順
Methyl 2-(3-mercaptophenyl)acetate (0.55 g, 3.0 mmol) was dissolved in 10 mL acetonitrile and potassium nitrate (0.76 g, 7.5 mmol) was added and the reaction mixture cooled to 0° C. To this suspension sulfuryl chloride was added (0.6 mL, 7.5 mmol) at 0° C. and the reaction mixture was let warm to room temperature and stirred overnight. A solution of saturated sodium bicarbonate was added followed by ethyl acetate (100 mL each). The organic layer was washed with brine, dried over sodium sulfate and concentrated to afford methyl 2-(3-chlorosulfonylphenyl)acetate as an oil (0.59 g, 2.4 mmol, 79% yield). 1H NMR (CDCl3) 7.91 ppm, 2H, m; 7.60 ppm, 1H, d; 7.53 ppm, 1H, t; 3.73 ppm, 2H, s; 3.72 ppm, 3H, s.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07531556B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-08aff3d6ddee47f89a330fbb070def5f |
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| 出典メモ | uspto-grants-2009_05 |
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