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Dicyclohexylamine → 1-Phenyl-4-cyano-5-(dicyclohexylaminosulfonylureido)pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylamine | HCID 7582 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 反応物 | 5-Amino-1-phenyl-1H-pyrazole-4-carbonitrile | HCID 79256 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Phenyl-4-cyano-5-(dicyclohexylaminosulfonylureido)pyrazole | HCID 18993711 | 87% |
反応手順
4.4 ml (50 mmol) of chlorosulfonyl isocyanate were added to a solution of 9.2 g (50 mmol) of 1-phenyl-4-cyano-5-aminopyrazole in 100 ml of methylene chloride. Stirring was carried out for 30 minutes at about 20° C., after which a solution of 7.5 ml (60 mmol) of triethylamine and 10 ml (50 mmol) of dicyclohexylamine in 50 ml of methylene chloride was slowly added dropwise. After the end of the addition, stirring was continued for a further hour and hydrolysis was then carried out with 200 ml of water. The organic phase was separated off and was worked up in a conventional manner to give the product. Yield: 87%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05486618 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-892ac24930964938b65e8098dccb8a46 |
| 出典メモ | uspto-grants-1996_01 |