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p-Toluenesulfonic acid monohydrate → 1-[5-[(Z)-2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-thiophen-2-yl]-piperidin-4-yl diethylamino-acetate p-toluenesulfonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | (Z)-2-(3,4-dimethoxyphenyl)-3-(5-(4-hydroxypiperidin-1-yl)thiophen-2-yl)acrylonitrile | HCID 16757522 | — |
| 反応物 | Glycine, N,N-diethyl-, sodium salt (1:1) | HCID 23670834 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-[5-[(Z)-2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-thiophen-2-yl]-piperidin-4-yl diethylamino-acetate p-toluenesulfonate | HCID 11964787 | 37.7% |
反応手順
Compound 6 (480 mg) was dissolved in toluene (100 mL), and N,N-diethylglycin sodium salt (296 mg) and p-toluenesulfonic acid monohydrate (490 mg) were added to the solution, followed by stirring under reflux for 5 hours. The solvent was evaporated to dryness, and the residue was purified by silica gel column chromatography (CHCl3-MeOH), to thereby yield the target product (yield: 237 mg, 37.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08697742B2 |
| 出典データセット | uspto-grants-2014_04 |
| ORD ID | ord-34166a4ba0b14e9ea5e855b7b0ac7241 |
| 出典メモ | uspto-grants-2014_04 |