化工社化工社 化学情報印刷レポート · 研究参考用
Benzaldehyde, 4-octyl- → HCID 178442645、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzaldehyde, 4-octyl- | HCID 2734685 | — |
| 反応物 | Phosphinic acid, (3-aminopropyl)(diethoxymethyl)-, ethyl ester | HCID 10422382 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178442645 | HCID 178442645 | 47.4% |
反応手順
A mixture of 98.5 mg (0.389 mmol) of ethyl 3-aminopropyl (diethoxymethyl)phosphinate (from Step B) and 84.9 mg (0.389 mmol) of 4-octylbenzaldehyde in 1 mL of MeOH at rt was treated with 12.2 mg (0.194 mmol) Na(CN)BH3. The resulting reaction mixture was stirred at rt for 16 hr. The reaction was quenched with 0.5 mL of 12 N HCl, then heated up to 80° C. for 1 hr. The mixture was cooled and concentrated. HPLC purification (LC-2) afforded 60 mg (47%) of the title compound: 1H NMR (500 MHz, CD3OD) δ 0.88 (t, J=7.1, 3H), 1.25-1.33 (m, 10H), 1.59-1.66 (m, 4H), 1.90-1.96 (m, 2H), 2.63 (t, J=7.7, 2H), 3.09 (t, J=6.9, 2H), 4.12 (s, 2H), 7.03 (d, J=505.6, 1H), 7.27 (d, J=8.0, 2H), 7.38 (d, J=8.0, 2H); LC-1: 3.02 min; ESI-MS 326 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07351725B2 |
| 出典データセット | uspto-grants-2008_04 |
| ORD ID | ord-430a0edb506540d7a71620ba4488423a |
| 出典メモ | uspto-grants-2008_04 |