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(Phenylmethyl)hydrazine → (+/-)-3-Benzyl-3,4-diazabicyclo[4.1.0]heptane-2,5-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (Phenylmethyl)hydrazine | HCID 11157 | — |
| 反応物 | 3-Oxabicyclo(3.1.0)hexane-2,4-dione | HCID 2734721 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (+/-)-3-Benzyl-3,4-diazabicyclo[4.1.0]heptane-2,5-dione | HCID 10680232 | 29.8% |
反応手順
In 150 ml of acetonitrile was dissolved 42 g (374 mmol) of 1,2-cyclopropanedicarboxylic acid anhydride, and to the solution was added dropwise a solution of 45.8 g (374 mmol) of benzylhydrazine in 50 ml of acetonitrile, and the mixture was heated under reflux for 15 hours. The solvent was removed by distillation under reduced pressure, and the residue was purified by silica gel column chromatography. Crystallization from ethyl acetate gave 24.1 g (29.7%) of the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05418232 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-fa4eb2357689441a9fe836f52ad71c32 |
| 出典メモ | uspto-grants-1995_05 |