化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → N-benzyl-3-chloro-N-(2-methylallyl)-1,2-dihydrocyclobutabenzene-1-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium tetrametaphosphate | HCID 25951 | — |
| 反応物 | 2-Chlorobicyclo(4.2.0)octa-1(6),2,4-triene-7-carboxylic acid | HCID 10261768 | — |
| 反応物 | N-Benzyl-2-methylprop-2-en-1-amine | HCID 13788484 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-benzyl-3-chloro-N-(2-methylallyl)-1,2-dihydrocyclobutabenzene-1-carboxamide | HCID 70664766 | 72% |
反応手順
To a solution of 3-chloro-1,2-dihydrocyclobutabenzene-1-carboxylic acid (7.67 mmol, 1.4 g) in DCM (20 ml) was added N-benzyl-2-methylprop-2-en-1-amine (11.50 mmol, 1.854 g), triethylamine (15.33 mmol, 2.131 ml, 1.552 g) and cyclophos (50 wgt % solution in EtOAc) (9.20 mmol, 2.74 ml, 2.93 g). The mixture was stirred at ambient temperature overnight then cyclophos (50 wgt % solution in EtOAc) (0.5 ml) added and the mixture stirred for a further 1 hr. The mixture was diluted with DCM (10 ml), washed with 2 N HCl (20 ml) then 2 N NaOH (20 ml), dried over Na2SO4, filtered and concentrated under reduced pressure to afford N-benzyl-3-chloro-N-(2-methylallyl)-1,2-dihydrocyclobutabenzene-1-carboxamide as a brown oil (1.8 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08729274B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-4416d0814c924df4a2ef4dfd1f42386c |
| 出典メモ | uspto-grants-2014_05 |