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Sodium Carbonate → HCID 178472137、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Hydrazinecarboxaldehyde, 1-methyl- | HCID 12962 | — |
| 反応物 | Ethyl 2-(2,3-Difluoro-5-iodobenzoyl)-3-ethoxy-2-propenoate | HCID 69879816 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178472137 | HCID 178472137 | — |
反応手順
A solution of 1-formyl-1-methylhydrazine (0.217 g) in toluene (0.5 mL) is added to a solution of ethyl 2-(2,3-difluoro-5-iodobenzoyl)-3-ethoxy-2-propenoate (Preparation 21, 1.00 g) in toluene (2.5 mL) at 33° C. After stirring at ambient temperature for 20 minutes, a precipitate formed and an additional 1.5 mL of toluene is added. After an additional 1.75 h, solid anhydrous Na2CO3 (0.285 g) is added and the reaction mixture is heated to reflux. After 1 h, the reaction mixture is concentrated at reduced pressure and the residue suspended in 8 mL of water which is used as is in the following step. Physical characteristics: MS (ESI+) m/z 419 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06624159B2 |
| 出典データセット | uspto-grants-2003_09 |
| ORD ID | ord-9e8961366057427c8c487a5a6fc100ca |
| 出典メモ | uspto-grants-2003_09 |