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Water → HCID 70288966、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-(Methylsulfonyl)benzaldehyde | HCID 220376 | — |
| 反応物 | Methyl 5,6-difluoro-2-methylindene-3-acetate | HCID 12052144 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 70288966 | HCID 70288966 | — |
反応手順
Methyl 5,6-difluoro-2-methylindene-3-acetate (1.19 g, 5.0 mmol) from Example 2, Part E and of p-methylsulfonylbenzaldehyde (0.76 g, 5.0 mmol) in dry pyridine (10 ml) are treated under nitrogen with Triton B (5.0 g, 5.1 mmol). The deeply colored solution is kept overnight. Water (2 ml) is added, the solution is stirred for 15 minutes and is poured into excess water. The mixture is extracted with ether (2×50 ml). The aqueous phase is added to 10% HCl-ice. The solution of the precipitate is extracted into methylene chloride and is dried (MgSO4). The solvent is evaporated to leave an orange solid which is recrystallized from benzene to give (Z)-5,6-difluoro-2-methyl-1-(p-methylsulfonylbenzylidene)-indene-3-acetic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06028116 |
| 出典データセット | uspto-grants-2000_02 |
| ORD ID | ord-5f0ad651339a4210bcd234822b133a3f |
| 出典メモ | uspto-grants-2000_02 |