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Oxalyl chloride → N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | N'-tert-butylbenzohydrazide | HCID 299436 | — |
| 反応物 | 4,4,4-Trifluoro-3-methyl-2-butenoic acid | HCID 5708835 | — |
| 反応物 | beta-Trifluoromethylcrotonyl chloride | HCID 86745869 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine | HCID 70294050 | — |
反応手順
N'-t-butyl-N-benzoylhydrazine (1.0 g,) in 2 ml toluene was added dropwise to a solution of beta-trifluoromethylcrotonyl chloride (prepared by addition of oxalyl chloride (1.3 g) to a solution of 1.5 g beta-trifluoromethylcrotonic acid in 5 ml toluene at 23° C.). After 30 minutes at 23° C., the reaction mixture was partitioned between saturated aqueous sodium bicarbonate (20 ml) and ether (20 ml). The ether layer was evaporated under reduced pressure to about 10 ml and the excess hydrazine was removed by filtration. The filtrate was evaporated to give N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine as a colorless oil.
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-1eddb448ff674889bf5ee66e8cf10c6f |
| 出典メモ | uspto-grants-1995_06 |