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Water → 1,1-dimethylethyl(3S)-3-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-(Trifluoromethyl)benzenesulfonyl chloride | HCID 2777399 | — |
| 反応物 | (S)-1-Boc-3-methylpiperazine | HCID 7023035 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,1-dimethylethyl(3S)-3-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinecarboxylate | HCID 59152113 | 105.2% |
反応手順
To a solution of 1,1-dimethylethyl (3S)-3-methyl-1-piperazinecarboxylate (2.05 g, 10.24 mmol) in DCM (50 ml) was added DIPEA (2.68 ml, 15.35 mmol) and the mixture stirred at room temperature for 10 minutes before addition of 4-(trifluoromethyl)benzenesulfonyl chloride (3.00 g, 12.28 mmol) at 0° C. The resultant mixture stirred under an atmosphere of Argon for 16 hours before addition of water (50 ml) and DCM (30 ml). The layers were separated using a hydrophobic frit and the organic layers concentrated to dryness giving the title compound (4.4 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08530478B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-7f9e4259d82f4eedb26b34a740a976fc |
| 出典メモ | uspto-grants-2013_09 |