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3-Chloro-1-butene → 1-(1-Methyl-2-propenyloxy)-5-methyl-2-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Chloro-1-butene | HCID 11242 | — |
| 反応物 | 6-Nitro-m-cresol | HCID 12788 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(1-Methyl-2-propenyloxy)-5-methyl-2-nitrobenzene | HCID 13560293 | — |
反応手順
24 g of sodium hydride was added in portions to a stirred mixture of 153 g of 5-methyl-2-nitrophenol and 500 ml of DMSO. Then 135.7 g of 3-chloro-1-butene was added drop-by-drop (over 5 minutes) to the stirred mixture, which then was stirred at reflux (79°-81° C.) for 24 hours. Then the mixture was made basic with 50% aqueous sodium hydroxide, poured over ice water and extracted with methylene chloride. The extract was washed with cold water, dried (MgSO4), filtered and stripped of solvent, to give 1-(1-methyl-2-propenyloxy)-5-methyl-2-nitrobenzene (1A), as a dark-colored syrup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04558040 |
| 出典データセット | uspto-grants-1985_12 |
| ORD ID | ord-89f1cfebad004de6b9345d10f5f19162 |
| 出典メモ | uspto-grants-1985_12 |