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2,3,4-Trimethoxybenzaldehyde → 5-Methoxy-2-methyl-1-(2,3,4-trimethoxybenzylidene)-3-indenyl acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3,4-Trimethoxybenzaldehyde | HCID 75006 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Methyl 5-methoxy-2-methyl-3-indenylacetate | HCID 53634864 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Methoxy-2-methyl-1-(2,3,4-trimethoxybenzylidene)-3-indenyl acetic acid | HCID 54456864 | — |
反応手順
To a solution of methyl 5-methoxy-2-methyl-3-indenylacetate 8.7 g (0.037 mol) and 2,3,4-trimethoxybenzaldehyde, 7.99 g (1.1 equivalent) is added 16+ ml (2.0+ equivalents) of 25% methanolic sodium methoxide. The mixture is stirred at reflux under nitrogen for 2 hours. An equal volume of water is added dropwise and refluxing continues for 30 min. The solution is cooled, diluted with water and extracted with ether (3×). Residual ether is blown off with nitrogen, and then the aqueous solution is acidified with 50% glacial acetic acid. The precipitated product is collected and washed thoroughly with water. The crude product is crystallized to give 5-methoxy-2-methyl-1-(2,3,4-trimethoxybenzylidene)-3-indenyl acetic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06063818 |
| 出典データセット | uspto-grants-2000_05 |
| ORD ID | ord-c8d6ac03cf494bef87c4032218104125 |
| 出典メモ | uspto-grants-2000_05 |