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Cyclobutanone → tert-Butyl cyclobutylidenecarbazate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclobutanone | HCID 14496 | — |
| 反応物 | tert-Butyl carbazate | HCID 70091 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | tert-Butyl cyclobutylidenecarbazate | HCID 45092398 | 81.2% |
反応手順
The reaction mixture of cyclobutanone (15 g, 214 mmol) and hydrazinecarboxylic acid tert-butyl ester (28.3 g, 214 mmol) in hexane (225 mL) was heated to reflux for 2 hours. After cooling down, a precipitate formed and the solid was filtered under vacuum. Isopropanol (10 mL) and hexane (100 mL) were added to the solid and the mixture was put on the rotary evaporator under vacuum until a slurry was generated. After filtration, the solid was washed with hexane twice and dried in vacuo to afford N′-cyclobutylidene-hydrazinecarboxylic acid tert-butyl ester (32 g, 81%) as white solid which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728029B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-8077ea87bc5b4e968bb24e3cbfde846c |
| 出典メモ | uspto-grants-2010_06 |