化工社化工社 化学情報印刷レポート · 研究参考用
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 86705049、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | Diethyl (methanesulfonylmethyl)phosphonate | HCID 533797 | — |
| 反応物 | HCID 86705048 | HCID 86705048 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 86705049 | HCID 86705049 | — |
反応手順
To a solution of diethyl methylsulfonylmethylphosphonate (1.05 g, 4.56 mmol) in CH3CN (30 mL) at RT was added LiCl (0.16 g, 3.80 mmol) and DBU (2.40 g, 9.56 mmol). After 5 min, a solution of methyl 2-(4-chlorophenyl)-2-(4-formyl-1H-indol-1-yl)butanoate (1.35 g, 3.80 mmol) in CH3CN (10 mL) was added dropwise. The resulting mixture was stirred for 4 hours at RT. Then it was diluted with DCM (50 mL) and the organic layer was washed with water (30 mL), dried over Na2SO4, filtered. After removal of the solvent, the residue was purified via column chromatography (0-30% EtOAc/hexanes) to provide the title compound. LC/MS m/z=432.0[M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08933113B2 |
| 出典データセット | uspto-grants-2015_01 |
| ORD ID | ord-f6fcc6df39154dfcadaca6fd844ee9f9 |
| 出典メモ | uspto-grants-2015_01 |