関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Pyridinecarbonyl chloride, hydrochloride (1:1) | HCID 88438 | — |
| 反応物 | N'-tert-butylbenzohydrazide | HCID 299436 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N'-t-butyl-N-benzoyl-N'-nicotinoylhydrazine | HCID 15767543 | — |
反応手順
A solution of N'-t-butyl-N-benzoylhydrazine (2.0 g) and nicotinoyl chloride hydrochloride in 20 ml of methylene chloride at 23° C. was treated dropwise with triethylamine (4 ml). The reaction mixture was stirred at 23° C. for 0.5 hours. Solids were removed by filtration. The filtrate was diluted with 10N HCl and ether. The layers were separated and the organic layer was washed with 10N HCl. The aqueous layer was neutralized with solid sodium bicarbonate and extracted with ether. The ether extracts were treated with charcoal and then dried with magnesium sulfate. Evaporation of solvents afforded a yellow oil which was chromatographed on silica gel using as eluant a mixture of 10% CH3OH, 40% CH2Cl2, 50% Et2O to afford N'-t-butyl-N-benzoyl-N'-nicotinoylhydrazine as a yellow foam: m.p. 60°-63° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05424333 |
|---|
| 出典データセット | uspto-grants-1995_06 |
|---|
| ORD ID | ord-7040c1e3278a4d979435f82d9d30012e |
|---|
| 出典メモ | uspto-grants-1995_06 |
|---|