関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (2,6-Dicyanophenyl)boronic acid | HCID 22571817 | — |
| 反応物 | HCID 22970630 | HCID 22970630 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Water 1,2-dimethoxyethane | HCID 18180031 | — |
| 生成物 | HCID 57297799 | HCID 57297799 | 65.5% |
反応手順
To a mixture of 2,6-dicyanobenzene boronic acid (0.516 g) and anhydrous K2CO3 (0.52 g) in DME/H2O (10 mL/0.5 mL) under N2 was added N-(2,6-dichlorobenzoyl)-O-(trifluoromethanesulfonyl)-L-tyrosine methyl ester (0.5 g), The catalyst Pd(PPh3)4 (0.1 g) was added and the mixture was heated at 80° C. for 5 h. The mixture was cooled, diluted with EtOAc and washed successively with water and brine. The organic layer was dried (MgSO4), evaporated, and the residue was purified by column chromatography (silica gel; eluent: EtOAc/hexane 3/1)) to yield 325 mg of N-(2,6-dichlorobenzoyl)-4-(2-cyano-6-carbamoyl-phenyl)-L-phenylalanine methyl ester. ESMS: m/z 496 (MH+), 494 (M−H)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06521666B1 |
|---|
| 出典データセット | uspto-grants-2003_02 |
|---|
| ORD ID | ord-8f4fa70b6a35419191ab8b802c09e400 |
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| 出典メモ | uspto-grants-2003_02 |
|---|
