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Hexane → Dimethyl 3-phenylthiocyclobutane-1,2-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Phenyl Vinyl Sulfide | HCID 74572 | — |
| 反応物 | Dimethyl maleate | HCID 5271565 | — |
| 反応物 | Ethyl aluminium dichloride | HCID 16686341 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Dimethyl 3-phenylthiocyclobutane-1,2-dicarboxylate | HCID 86746186 | — |
反応手順
To a solution of dimethyl maleate (0.50 mL, 4 mmol) and phenyl vinyl sulfide (0.52 mL, 4 mmol) in 17 mL of 1,2-dichloroethane under nitrogen atmosphere, was added 1 equivalent (4 mL of a 1 M solution in hexane) of ethylaluminum dichloride. The resultant solution was heated at 85° C. for 18 h and then diluted with 75 mL of methylene chloride. The methylene chloride solution was washed three times with saturated aqueous ammonium chloride and once with brine, dried over anhydrous sodium sulfate, filtered and concentrated to give 0.98 g of the title compound; EI-MS, m/e (rel intensity): 280 (M+, 14), 136 (100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246931 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-cfd97c6b760d447ab41eb374f30d7b03 |
| 出典メモ | uspto-grants-1993_09 |