関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 4-Mesylphenylacetic acid | HCID 572345 | — |
| 反応物 | 2-(2-Nitro-4,5-dichlorophenyl)-N-methyl-N-[(+/-)-trans-2-(1-pyrrolidinyl)-7-nitro-1,2,3,4-tetrahydronaphth-1-yl]acetamide | HCID 22879436 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 2-(4-Methylsulfonylphenyl)-N-methyl-N-[(1S)-1-(3-nitrophenyl)-2-(1-pyrrolidinyl)ethyl]acetamide | HCID 11385274 | — |
反応手順
This compound was prepared via the general DCC/pyr coupling procedure from 8 (0.5138 g, 2.061 mmol), 4-methylsulfonylphenylacetic acid (0.8825 g, 4.119 mmol), DCC(0.8771 g, 4.251 mmol), and pyridine (0.34 mL, 4.245 mmol). The crude product was gravity column chromatographed eluting with CHCl3:2% NH3 before it was converted to the HCl salt with 1.0 M HCl in Et2O and crystallized from MeOH to yield 14 HCl.(0.4695 g, 47%): m.p. (HCl salt) 276-277° C.; 1H NMR (HCl salt, DMSO-d6) δ2.0 (br s, 4H, —CH2CH2—), 2.92 (s, 3H, —NCH3), 3.2 (s, 3H, —SO2CH3), 3.2-4.3 (complex, 8H, 4 —CH2—), 6.25 (m, 1H, —CH—), 7.61 (d, J=7.2 Hz, 2H, aromatic), 7.75 (m, 2H, aromatic), 7.89 (d, J=7 Hz, 2H, aromatic), 8.12 (s, 1H, aromatic), 8.25 (m, 1H, aromatic). MS(FAB) m/z 446. Anal. (C, H, N) C22H27N3O5S HCl.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06750216B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-fcdaa121866d479688af9d18e13d5a7e |
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| 出典メモ | uspto-grants-2004_06 |
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