関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | Ethyl (2-ethylphenoxy)acetate | HCID 21986411 | — |
| 生成物 | Ethyl 2-(4-(chlorosulfonyl)-2-ethylphenoxy)acetate | HCID 21986343 | 70% |
反応手順
To a 250ml round-bottom flask containing chlorosulfonic acid (30ml) cooled to 0° C. was added ethyl (2-ethylphenoxy)acetate (7.2g, 34.6mmoles) dropwise. Once the addition was complete the ice-bath was removed and the reaction was allowed to warm to room temperature at which the reaction was stirred for 3hours. The reaction was then slowly added to ice and, once the excess chlorosulfonic acid was quenched, the mixture was diluted with CH2Cl2(200ml). The phases were separated and the aqueous fraction washed with CH2Cl2twice. The combined organic fractions were dried over Na2SO4and filtered and concentrated in vacuo to yield 7.2g (70%) of crude product. The crude product was used with no purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07449468B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-3f77c5b4fc1248f6a579fbef01fdec08 |
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| 出典メモ | uspto-grants-2008_11 |
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