化工社化工社 化学情報印刷レポート · 研究参考用
Trityl chloride → Methyl-12-trityloxy-dodecanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Methyl 12-hydroxydodecanoate | HCID 522424 | — |
| 反応物 | Methyl 6-trityloxy-hexanoate | HCID 67198977 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | Methyl-12-trityloxy-dodecanoate | HCID 67200799 | 40% |
反応手順
The synthesis procedure of 15a was followed. Trityl chloride (1412 mg, 5.1 mmol), 14c (583 mg, 2.5 mmol), and pyridine (10 mL) were used and the reaction was prolonged to 3 days. The filtration step was omitted, instead the crude material was purified by flash column chromatography (10% EtOAc in hexanes) yielding 477 mg (40%) of a pale yellow oil 15c. 1H-NMR (400 MHz, CDCl3, δH ppm): 7.44 (6H, m, p-Ar), 7.28 (6H, m, m-Ar), 7.21 (3H, m, o-Ar), 3.66 (3H, s, CO2CH3), 3.03 (2H, t, 3JH—H=6.6 Hz, H)—CH2), 2.29 (2H, t, 3JH—H=7.5 Hz, CH2CO2), 1.55-1.65 (4H, m, 2CH2), 1.10-1.39 (14H, m, 7CH2). HRMS (EI): m/z calcd 472.2977 (C32H40O3), found 472.2968 [M]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08623326B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-97903a68f3f54b51a3bbcb210323c15d |
| 出典メモ | uspto-grants-2014_01 |