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Acetophenone → 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-2-(1-phenyl-1-ethylidene)hydrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetophenone | HCID 7410 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide | HCID 56942873 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-[2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetyl]-2-(1-phenyl-1-ethylidene)hydrazine | HCID 86689361 | 87.5% |
反応手順
To a 50 mL volume two-necked flask, 3.0 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetohydrazide ((12-1)-(11)-39), 20 ml of THF (anhydrous), 1.73 g of acetophenone and 780 mg of acetic acid were added under a nitrogen atmosphere, and the mixture was stirred for 6 hours under reflux. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. Water was added to the residue and the resultant was extracted with t-butyl methyl ether. The organic layer was concentrated under reduced pressure and hexane was added thereto. The precipitated crystals were collected by filtration and dried to give 3.77 g of 1-[2-(2,6-diethyl-4-methylphenyl)-2-oxoacetyl]-2-(1-phenyl-1-ethylidene)hydrazine ((40-a)-(14)-7).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08884010B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-1e9b6b45e51847d59ef193e706f32213 |
| 出典メモ | uspto-grants-2014_11 |