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Methanol → N-(4-chlorobutyl)-4-fluoro-N-(4-fluorophenyl)benzenamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Dimethyl Sulfide | HCID 1068 | — |
| 反応物 | Borane | HCID 6331 | — |
| 反応物 | 4-chloro-N,N-bis(4-fluorophenyl)butanamide | HCID 15087788 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(4-chlorobutyl)-4-fluoro-N-(4-fluorophenyl)benzenamine | HCID 14722551 | 91.5% |
反応手順
To a stirred and cooled (0° C.) solution of 48 parts of 4-chloro-N,N-bis(4-fluorophenyl)butanamide in 108 parts of tetrahydrofuran were added 240 parts of a solution of borane, compound with thiobismethane, in tetrahydrofuran. After stirring overnight at room temperature, the reaction mixture was decomposed with 160 parts of methanol. After evaporation, the residue was purified by column chromatography over silica gel using a mixture of triohloromethane and petroleum ether (20:80 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 32.5 parts (91.5%) of N-(4-chlorobutyl)-4-fluoro-N-(4-fluorophenyl)benzenamine as a residue (int. 70).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04968684 |
| 出典データセット | uspto-grants-1990_11 |
| ORD ID | ord-1d71af31ba654ed88325e25163b9a251 |
| 出典メモ | uspto-grants-1990_11 |