化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 10,11-Dihydro-10-(4-nitrobenzoyl)dibenz[b,f][1,4]thiazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Nitrobenzoyl chloride | HCID 8502 | — |
| 反応物 | 10,11-Dihydrodibenzo(b,f)(1,4)thiazepine | HCID 12310482 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 10,11-Dihydro-10-(4-nitrobenzoyl)dibenz[b,f][1,4]thiazepine | HCID 54570072 | 112.6% |
反応手順
To a solution of 1.6 g of 10,11-dihydrodibenz[b,f][1,4]thiazepine in 30 ml of dichloromethane is added 0.1 g of 4-(N,N-dimethylamino)pyridine, 4 ml of triethylamine and 1.0 g of 4-nitrobenzoyl chloride and the mixture is stirred for 16 hours. The mixture is poured into ice-water and extracted with 3×150 ml of dichloromethane. The combined organic extract is washed with water, 2N HCl, 2N Na2CO3, water and dried (MgSO4). The solvent is removed in vacuo and the product (2.6 g) purified by chromatography on silica is gel with hexane-ethyl acetate (4:1) as eluent to give 2.2 g of crystals, m.p. 147°-149° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05869483 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-be832396dc934b20a7511ec1baf80991 |
| 出典メモ | uspto-grants-1999_02 |