化工社化工社 化学情報印刷レポート · 研究参考用
1-Iodopentane → N-benzyl-N'-[3,5-bis(trifluoromethyl)benzoyl]-N-({4-[(pentyloxy)methyl]cyclohexyl}methyl)sulfamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Iodopentane | HCID 12335 | — |
| 反応物 | 2,6-Di-tert-butylpyridine | HCID 68510 | — |
| 反応物 | N-benzyl-N'-[3,5-bis(trifluoromethyl)benzoyl]-N-{[4-(hydroxymethyl)cyclohexyl]methyl}sulfamide | HCID 22574483 | — |
| 触媒 | Silver(I) trifluoromethanesulfonate | HCID 76223 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-benzyl-N'-[3,5-bis(trifluoromethyl)benzoyl]-N-({4-[(pentyloxy)methyl]cyclohexyl}methyl)sulfamide | HCID 22574478 | 73.9% |
反応手順
Intermediate (4) (27.6 mg, 50 μmole, 1.0 eq) was dissolved in dichloromethane (250 μL), after which 2,6-di-t-butyl pyridine (36 μL, 160 μmole, 3.2 eq), silver triflate (38.5 mg, 150 μmole, 3.0 eq) and iodopentane (23 μL, 175 μmole, 3.5 eq) were added. After 45 minutes the reaction mixture was directly purified to give 23 mg of the title compound. 1H NMR (500 MHz, DMSO-d6): δ 8.45 (s, 2H), 8.15 (s, 1H), 7.36 (d, 2H), 7.24 (t, 2H), 7.17 (t, 1H), 4.39 (s, 2H), 3.30 (water), 3.23 (t, 2H), 3.01 (d, 2H), 2.92 (d, 2H), 2.48 (DMSO), 1.61 (m, 2H), 1.54 (m, 2H), 1.41 (m, 2H), 1.34-1.19 (m, 6H), 0.82 (t, 3H), 0.62 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06852738B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-a8255898e3c043f2be177310735149d0 |
| 出典メモ | uspto-grants-2005_02 |