関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Diazonio-1-ethoxyprop-1-en-1-olate | HCID 53440922 | — |
| 反応物 | HCID 178438709 | HCID 178438709 | — |
| 触媒 | Acetic acid, rhodium(2+) salt | HCID 21674 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178438728 | HCID 178438728 | 88.4% |
反応手順
A mixture of 3′-fluoro-4′-{[4-(trans-4-hydroxycyclohexyl)-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (3.0 g), rhodium(II) acetate (dimer) (0.027 g) and toluene (30 mL) was heated to 80° C. under an argon atmosphere, a solution of ethyl 2-diazopropionate (3.2 g) in toluene (30 mL) was added dropwise, and the mixture was stirred at 80° C. for 10 min. A solution of ethyl 2-diazopropionate (1.6 g) in toluene (10 mL) was added, and the mixture was stirred at 80° C. for 10 min. The reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography to give the title compound as a colorless solid (3.2 g, 88%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08921379B2 |
|---|
| 出典データセット | uspto-grants-2014_12 |
|---|
| ORD ID | ord-cfefed01ceba4973baf51a786e931e2b |
|---|
| 出典メモ | uspto-grants-2014_12 |
|---|