化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Methyl triflate | HCID 9526 | — |
| 反応物 | 3-Cyano-4-dimethylamino-benzoic acid methyl ester | HCID 59847657 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate | HCID 86621519 | 69% |
反応手順
To a stirred solution of 6.16 g (30.2 mmol) 3 and 110 ml dichloromethane were added 50.0 g (302 mmol) methyltriflate (Aldrich) drop wisely. The reaction mixture was stirred over night and diethylether was added. After evaporation of one third of the solvent volume the desired compound precipitates and the rest of the solvent were decanted. The solid was washed extensively (ten times) with large amounts of diethylether. The solid was dried by use of oil pump vacuum and purified by (C-18) RP-column chromatography (acetonitril/water—gradient 1:99 to 80:20). The desired compound 4 was obtained in 69% yield (20.8 mmol, 7.68 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08557776B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-14848f56a14a460f8cd5383286b8ca90 |
| 出典メモ | uspto-grants-2013_10 |