関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Acetone Cyanohydrin | HCID 6406 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 8,9-dihydro-3-nitro-5H-benzocyclohepten-5-one | HCID 20094732 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-nitro-5-oxo-6,7,8,9-tetrahydro [5H] benzocycloheptene-7-carbonitrile | HCID 54523296 | — |
反応手順
A mixture of 50 g of 3-nitro-8,9-dihydro [5H] benzocycloheptene-5-one, 1200 ml of methanol, 120 ml of tetrahydrofuran, 100 ml of a 10% aqueous potassium carbonate and 50 ml of acetone cyanhydrin under nitrogen was refluxed for an hour in a bath at 90° C. and the mixture was concentrated to about 200 ml under reduced pressure. The mixture was cooled to 20° C. and was extracted with methylene chloride. The organic phase was washed with water, dried and distilled to dryness under reduced pressure. The 58 g of brown oil residue were crystallized from 50 ml of methanol and the mixture was vacuum filtered to obtain 46 g of 3-nitro-5-oxo-6,7,8,9-tetrahydro [5H] benzocycloheptene-7-carbonitrile with a melting point of 107° C. and then 120° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04117164 |
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| 出典データセット | uspto-grants-1978_09 |
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| ORD ID | ord-2b0346b56d1d41af8c8e1dd4e1b2dc2c |
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| 出典メモ | uspto-grants-1978_09 |
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