関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 2-thiopheneglyoxylate | HCID 77693 | — |
| 反応物 | (3-Methylbutyl)hydrazine | HCID 18696583 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | [(3-Methyl-butyl)-hydrazono]-thiophen-2-yl-acetic acid ethyl ester | HCID 72562995 | 47.1% |
反応手順
To a solution of oxo-thiophen-2-yl-acetic acid ethyl ester (1d) (3.97 g, 21.6 mmol) in absolute ethanol (100 mL), (3-Methyl-butyl)-hydrazine (2b) (2.0 g, 19.6 mmol) was added. The mixture was stirred at 80° C. under N2 atmosphere for 2-25 hours. The reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography on silica gel to give the desired product (3d) (2.48 g) that was directly used in the next step. LC-MS (ESI+): m/e 269.2 [M+1]+, 537.4 [2M+1]+, 559.0 [2M+Na]+ (exact ms: 268.12).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07425552B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-87f0c78e6581409aafe2d4313913c391 |
|---|
| 出典メモ | uspto-grants-2008_09 |
|---|