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Diisopropylethylamine → HCID 178484845、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-(Trifluoromethyl)benzenesulfonyl chloride | HCID 2777399 | — |
| 反応物 | HCID 178484843 | HCID 178484843 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178484845 | HCID 178484845 | 77% |
反応手順
To 3 g (23.2 mmol) trans-4-Methylamino-cyclohexanol in 120 ml CH2Cl2 were added 4.2 ml (24.4 mmol, 1.05 eq) N,N-diisopropylethylamine followed by 5.96 g (24.4 mmol, 1.05 eq) 4-(trifluoromethyl)-benzenesulfonyl chloride in 50 ml CH2Cl2. The mixture was stirred at RT over night and the organic phase extracted with 1M KHSO4, followed by 5% NaHCO3 and brine. The combined organic phases were washed with brine, dried over Na2SO4 and evaporated. Column chromatography on silica gel with hexane:EtOAc 1:1 yielded 6.0 g (77%) trans-N-(4-Hydroxy-cyclohexyl)-N-methyl-4-trifluoromethyl-benzenesulfonamide as off-white solid, MS: 338 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858651B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-b85d099259e8475f8ee61f1318b3a6b9 |
| 出典メモ | uspto-grants-2005_02 |