関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bis(dichloromethyl) ether | HCID 558102 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | HCID 21278475 | HCID 21278475 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 4-formyl-[(2-propynyl)]-1H-pyrrole-2-carbonitrile | HCID 13605013 | 117% |
反応手順
A mixture of 2.36 g of aluminium chloride in 6 ml of anhydrous methylene chloride was cooled to -78° C. and 1.3 g of the product of Step A in solution in 8 ml of methylene chloride and 0.5 ml of nitromethane were added. 1.49 g of dichloromethyl ether in solution in 15 ml of methylene chloride were added at -55° C. and the reaction mixture was kept for 1 hour at -60° C., then allowed to return to 20° C., at which temperature it was held for 18 hours. It was poured into water, stirred, and neutralized to pH 7 by addition of 33 ml of 2N sodium hydroxide. Extraction was with methylene chloride and the extracts were washed with a 1M potassium bicarbonate solution, dried and concentrated to dryness to obtain 1.5 g of 4-formyl-[(2-propynyl)]-1H-pyrrole-2-carbonitrile which was washed with dupentane and dried to obtain 1.1 g of the said product melting at 97° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04737513 |
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| 出典データセット | uspto-grants-1988_04 |
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| ORD ID | ord-7fb0004cb91b482aa238ed594670f3e0 |
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| 出典メモ | uspto-grants-1988_04 |
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