関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 1,1,1-Triethoxypentane | HCID 70195 | — |
| 反応物 | HCID 178499531 | HCID 178499531 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | methyl [(4Z)-4-(1-ethoxypentylidene)-1-methyl-5-oxo-4,5-dihydro-1H-pyrazol-3-yl]acetate | HCID 86686093 | — |
反応手順
The mixture of the above obtained methyl (5-hydroxy-1-methyl-1H-pyrazol-3-yl)acetate (Compound of Formula (IV), 0.80 g) in acetonitrile (5 mL), glacial acetic acid (21 μl 0.1 equiv.) and BuC(OEt)3 (3 eq.) was heated at 70° C. for 1 h 15. The resulting red solution was concentrated in vacuo to afford a red syrup that was washed with cyclohexane and then dried in vacuo. Due to its relative instability, no further purification of methyl[(4Z)-4-(1-ethoxypentylidene)-1-methyl-5-oxo-4,5-dihydro-1H-pyrazol-3-yl]acetate was conducted (1.0 g, quantitative yield). MS (ESI+): 283.4; MS (ESI−): 281.3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08455485B2 |
|---|
| 出典データセット | uspto-grants-2013_06 |
|---|
| ORD ID | ord-8ddae73c475047ca9904455e40b28531 |
|---|
| 出典メモ | uspto-grants-2013_06 |
|---|