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Diisopropylethylamine → 1,1-dimethylethyl (2S)-4-{[2-bromo-5-(trifluoromethyl)phenyl]sulfonyl}-2-methyl-1-piperazinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Bromo-5-(trifluoromethyl)benzene-1-sulfonyl chloride | HCID 2778613 | — |
| 反応物 | tert-Butyl (2S)-2-methylpiperazine-1-carboxylate | HCID 10081508 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,1-dimethylethyl (2S)-4-{[2-bromo-5-(trifluoromethyl)phenyl]sulfonyl}-2-methyl-1-piperazinecarboxylate | HCID 66649471 | 103% |
反応手順
To a solution of 1,1-dimethylethyl(2S)-2-methyl-1-piperazinecarboxylate (1.18 g, 4.98 mmol) in dichloromethane (40 ml) was added DIPEA (2.70 ml, 15.45 mmol) and then 2-bromo-5-(trifluoromethyl)benzenesulfonyl chloride (1.613 g, 4.98 mmol). The reaction mixture was stirred for 1 h 20 min at room temperature, and then washed with water (50 ml), dried on a phase separation cartridge and concentrated under vacuum to give the crude title compound (2.5 g) used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093249B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-f876c7a341774aaaa67a8a4c5b16979b |
| 出典メモ | uspto-grants-2012_01 |