関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Mandelonitrile | HCID 10758 | — |
| 反応物 | 3,5-Dimethylpyridine | HCID 11565 | — |
| 反応物 | Benzoyl chloride, 3,6-dichloro-2-methoxy- | HCID 82609 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Cyano(phenyl)methyl 3,6-dichloro-2-methoxybenzoate | HCID 13206467 | — |
反応手順
Benzaldehyde cyanohydrin (13.3 grams; 0.100 moles), 3,5-lutidine (11 grams) and methylene chloride (100 ml) were placed in a 500 ml. 3-necked glass reaction flask equipped with a mechanical stirrer, thermometer, condenser and addition funnel. This mixture was cooled to 10° C. by means of an ice bath and 2-methoxy-3,6-dichlorobenzoic acid chloride (23.9 grams; 0.10 moles) was added dropwise with the temperature of the mixture maintained at 5°-10° C. After the addition of the acid chloride was completed, the reaction mixture was stirred for an additional three hours at room temperature. After the reaction was completed, the mixture was washed three times with water, dried over anhydrous magnesium sulfate, filtered and concentrated by distillation. The residue was heated to a temperature of 150° C. under vacuum from a vacuum pump. Then the residue was dissolved in cyclohexane, treated with nuchar, filtered and stripped dry to give an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04440567 |
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| 出典データセット | uspto-grants-1984_04 |
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| ORD ID | ord-9c4209d943364f8ca43ea4ab23b9381f |
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| 出典メモ | uspto-grants-1984_04 |
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