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Phosphonium, ((4-methylphenyl)methyl)triphenyl-, bromide (1:1) → 2,6-Diisopropyl-3-hydroxymethyl-4-(4-fluorophenyl)-5-[3-(4methyl-phenyl)propyl]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphonium, ((4-methylphenyl)methyl)triphenyl-, bromide (1:1) | HCID 11797662 | — |
| 反応物 | Methyl-2,6-diisopropyl-4-(4-fluorophenyl)-5-(2-oxoethyl)-3-pyridinecarboxylate | HCID 22005171 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 2,6-Diisopropyl-3-hydroxymethyl-4-(4-fluorophenyl)-5-[3-(4methyl-phenyl)propyl]pyridine | HCID 22004997 | — |
反応手順
The title compound was prepared from methyl-2,6-diisopropyl-4-(4-fluorophenyl)-5-(2-oxoethyl)-3-pyridinecarboxylate (Example 82, Step A) and 4-methylbenzyl triphenylphosphonium bromide according to the procedures described in Example 1, Steps F-H. 1H NMR (300 MHz, CDCl3): δ 7.08 (m, 4 H), 7.01 (d, J=8 Hz, 2 H), 6.85 (d, J=8 Hz, 2 H), 4.30 (s, 2 H), 3.39 (sept, J=6.6 Hz, 1 H), 3.13 (sept, J=6.6 Hz, 1 H), 2.41 (t, J=7 Hz, 2 H), 2.31 (s, 3 H), 2.27 (m, 2 H), 1.58 (m, 2 H), 1.31 (d, J=6.6 Hz, 6 H), 1.26 (d, J=6.6 Hz, 6 H), 1.15 (m, 1 H). FAB-MS: calcd for (C28H34FNO) 419, found 420 (M+H). Anal. Calcd for C28H34FNO: C, 80.15; H, 8.17; N, 3.34. Found: C, 80.33; H, 8.28; N, 3.22. mp 79-80° C. Rf=0.4 (20% ethyl acetate/hexane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06218431B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-bb4bea289c554795abf98ceac614cb51 |
| 出典メモ | uspto-grants-2001_04 |