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Acetic Acid → 4-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | (1,1'-Bicyclohexyl)-4-one | HCID 41690 | — |
| 反応物 | Phosphorohydrazidic acid, diethyl ester | HCID 143340 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester | HCID 85540745 | — |
反応手順
To a solution of 4-cyclohexylcyclohexanone (27.04 g) and acetic acid (3 ml) in CH2Cl2 (400 ml) was added a solution of diethyl phosphorohydrazidate (28.91 g) in CH2Cl2 (100 ml). The reaction was stirred at room temperature for 27 hours and then was concentrated under reduced pressure. Toluene was added (2X) and removed under reduced pressure in order to aid in the removal of acetic acid by codistillation. The residual yellow liquid was the product and was used without further purification. TLC Rf=0.52 (20% acetone in CH2Cl2, silica gel).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04917826 |
| 出典データセット | uspto-grants-1990_04 |
| ORD ID | ord-d71ebe81637245d1a89e1816f804b7cb |
| 出典メモ | uspto-grants-1990_04 |