化工社化工社 化学情報印刷レポート · 研究参考用
Ammonium Chloride → HCID 59497660、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Benzyltrimethylammonium hydroxide | HCID 66854 | — |
| 反応物 | 1,3-Dihydro-1-(1-methylvinyl)-2H-benzimidazol-2-one | HCID 100278 | — |
| 反応物 | Ethyl trans-2-hexenoate | HCID 5364778 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 59497660 | HCID 59497660 | 55% |
反応手順
To a solution of 1-isopropenyl-2-benzimidazolinone (2 g, 11.5 mmol) in DMF (10 mL) were added ethyl trans-2-hexenoate (2 g, 14 mmol) and the benzyltrimethylammonium hydroxide (40% in MeOH) (0.4 mL, 2.3 mmol) at room temperature. The solution was heated to 60 C for 12 hours. The solution was cooled down and sat.NH4Cl sol was added. The solution was extracted with EtOAc and the combined organic layer was dried with MgSO4 and filtered. The filtrate was concentrated and the residue was purified by CombiFlash with 20% EtOAc in Hexane to afford the desirable product 3-(3-Isopropenyl-2-oxo-2,3-dihydro-benzoimidazol-1-yl)-hexanoic acid ethyl ester (2 g, 55%) as an colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09150556B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-00b6d349062b4aa79ec4595566599d5b |
| 出典メモ | uspto-grants-2015_10 |