化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 12-(2,2,2-Trifluoroacetamido)dodecanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl trifluoroacetate | HCID 9893 | — |
| 反応物 | 12-Aminododecanoic Acid | HCID 69661 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 12-(2,2,2-Trifluoroacetamido)dodecanoic acid | HCID 21972557 | 97% |
反応手順
Methyl trifluoroacetate (200 μL, 1.99 mmoles) and triethylamine (184 μL, 1.32 mmoles) were added to a suspension of 12-aminododecanoic acid (300 mg, 1.32 mmoles) in methanol (2 mL). After the mixture was stirred vigorously for 18 h, 1 N HCl was added dropwise until the a pH of 2 was obtained. The reaction was added to ethyl acetate (20 mL) was washed with 1 N HCl (2×5 mL), dried over MgSO4, and concentrated in vacuo to yield the amide as a white solid (398 mg, 1.28 mmoles, 97%). LRMS: not performed. 1H NMR: spectrum is consistent with the predicted structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440988B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-e8d3cecc35b4472b9f4d76ad1a84f3e0 |
| 出典メモ | uspto-grants-2016_09 |