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2H-Azepine, 3,4,5,6-tetrahydro-7-methoxy- → 2-(alpha-Cyano-4-chlorobenzylidene)perhydroazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2H-Azepine, 3,4,5,6-tetrahydro-7-methoxy- | HCID 75657 | — |
| 反応物 | 4-Chlorobenzyl cyanide | HCID 241582 | — |
| 反応物 | Diazabicyclo[5.4.0]undec-5-ene | HCID 22258625 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(alpha-Cyano-4-chlorobenzylidene)perhydroazepine | HCID 70595042 | 67.6% |
反応手順
Agitate a mixture of 5.0 g of 4-chlorobenzyl cyanide, 5.5 g of caprolactim methyl ether and 0.5 g of diazabicyclo [5.4.0]undec-5-ene under nitrogen for 18 hours at 125°. Cool the thus-obtained reaction mixture to ambient temperature and then rub down the crystallizing residue with 20 ml of methyl alcohol before filtering to obtain 5.5 g of the title compound. Recrystallize this compound from methyl alcohol to obtain a product with a MP of 114° to 117°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04221788 |
| 出典データセット | uspto-grants-1980_09 |
| ORD ID | ord-34ac4d4d324f4803aaa661b56366f157 |
| 出典メモ | uspto-grants-1980_09 |