関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Aminothiophenol | HCID 14510 | — |
| 反応物 | Benzene, 1-fluoro-4-(trifluoromethyl)- | HCID 67873 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-{[4-(Trifluoromethyl)phenyl]sulfanyl}aniline | HCID 22175160 | — |
反応手順
To a stirred solution of 4-fluorobenzotrifluoride (9.85 g) and 4-aminothiophenol (7.51 g) in DMSO (60 mL), cooled in an ice bath, was added in one portion potassium t-butoxide (6.73 g). The resulting mixture was stirred at 0° C. for 10 minutes, then at 60° C. overnight. After cooling, the mixture was poured into water (600 mL) and the resulting mixture extracted with ether (2×200 mL). The organic phase was washed with 2N sodium hydroxide (50 mL), then with water (50 mL). After drying (MgSO4), the solvent was evaporated to give a brown solid. Recrystallization from hexane gave the title aniline as a yellow solid, m.p. 97-99° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06706740B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-2d142e8e4d7946b1ad94f4488202a711 |
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| 出典メモ | uspto-grants-2004_03 |
|---|
