化工社化工社 化学情報印刷レポート · 研究参考用
N-bromobutanimide → 2-Bromo-3,4-dimethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 3,4-Dimethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester | HCID 58256126 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Acetic acid chloroform | HCID 21584526 | — |
| 生成物 | 2-Bromo-3,4-dimethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester | HCID 66933907 | 75.2% |
反応手順
The product of step (b) (92 mg, 0.36 mmol) was dissolved in 4 mL of 1:1 HOAc/CHCl3 and treated with NBS (67 mg, 0.38 mmol). After stirring for ½ hour, the reaction was diluted with EtOAc (70 mL) was washed with water (3×30 mL) and 1M NaOH (2×30 mL). The organic solution was dried over MgSO4 and concentrated. The crude product was purified by silica gel chromatography (EtOAc/Hex) to give 90 mg of the sub-title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07893051B2 |
| 出典データセット | uspto-grants-2011_02 |
| ORD ID | ord-8c38dd3fcfb4405989ee390ff3a6c825 |
| 出典メモ | uspto-grants-2011_02 |