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Tetrahydrofuran → 2-Amino-3'-(tert-butoxycarbonylaminomethyl)benzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | tert-Butyl 3-bromobenzylcarbamate | HCID 11033439 | — |
| 反応物 | 2-amino-N-methoxy-N-methylbenzamide | HCID 11052242 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Amino-3'-(tert-butoxycarbonylaminomethyl)benzophenone | HCID 18315374 | — |
反応手順
A tetrahydrofuran (30 ml) solution of N-methyl-N-methyloxy-2-aminobenzamide (2.70 g) and N-tert-butoxycarbonyl-3-bromobenzylamine (2.86 g) was cooled to −78° C. To the solution was gradually added dropwise a hexane solution of n-butyl lithium (1.6 mol/L) (31 ml). To the mixture were then added water (70 ml) and acetic acid ethyl ester (70 ml). The organic layer was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off. The residual oily compound was purified by means of a silica gel column chromatography to give 2-amino-3′-(tert-butoxycarbonylaminomethyl)benzophenone as a yellow oily product (1.2 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06352982B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-6f193324f3ad43929deabd9c727960a6 |
| 出典メモ | uspto-grants-2002_03 |