関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | tert-Butyl mercaptan | HCID 6387 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-2-fluorobenzaldehyde | HCID 22019361 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-Bromo-2-(tert-butylthio)benzaldehyde | HCID 86662397 | 98.1% |
反応手順
A mixture of 3-bromo-2-fluorobenzaldehyde (5.0 g, 25 mmol), potassium carbonate (4.0 g, 30 mmol) and 2-methyl-2-propanethiol (5.5 mL, 49 mmol) in dry DMF (25 mL) was heated to 110° C. in a sealed tube for 16 h. The reaction mixture was cooled to RT, added to water (100 mL) and extracted with DCM (3×50 mL). The combined organic fractions were washed with water (50 mL), dried, and evaporated to afford 6.7 g (98%) of the crude title compound which was used without further purification. 1H NMR (300 MHz, CDCl3): δ 1.31 (s, 9H), 7.26-7.41 (m, 1H), 7.93-7.99 (m, 2H), 10.73 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08378104B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-9356c753a1e344abb506c2b0a4d487a4 |
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| 出典メモ | uspto-grants-2013_02 |
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