化工社化工社 化学情報印刷レポート · 研究参考用
Ammonium bifluoride → HCID 118380314、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium bifluoride | HCID 14935 | — |
| 反応物 | Cloperastine Hydrochloride | HCID 161104 | — |
| 反応物 | HCID 140689321 | HCID 140689321 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | HCID 22708839 | HCID 22708839 | — |
| 生成物 | HCID 118380314 | HCID 118380314 | 99.5% |
反応手順
Prepared according to Seki et al. Synlett 1995, 609-611. To a solution of tert-butyl 2-(((Z)-(1-(2-((tert-butoxycarbonyl)amino)thiazol-4-yl)-2-(((2R,3S)-2-(((2-((tert-butyldimethylsilyl)oxy)ethyl)amino)methyl)-4-oxoazetidin-3-yl)amino)-2-oxoethylidene)amino)oxy)-2-methylpropanoate (111 mg, 0.162 mmol) in DMF:NMP (2.7:1, 1.62 mL) was added ammonium fluoride hydrofluoride (37.0 mg, 0.648 mmol). After stirring for 65 h, the solution was diluted with water and extracted with EtOAc. The organic layer was dried over sodium sulfate and concentrated in vacuo to afford crude title compound (92 mg, 99%). The crude material was used directly in step 3. LCMS: R=0.76 min, m/z 571.3 (M+1) Method 2m_acidic.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09174978B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-7dc75cf636b5476cab09d566abb21a73 |
| 出典メモ | uspto-grants-2015_11 |