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4-Hydroxybenzaldehyde → 5-(4-Hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Hydroxybenzaldehyde | HCID 126 | — |
| 反応物 | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-(4-Hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 370541 | — |
反応手順
To a solution of 4-hydroxybenzaldehyde (20 g, 163 mmol) in water (250 mL) is added Meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione) (24.78 g, 171 mmol) as a slurry in water (250 mL) at 75° C. The reaction mixture is agitated for 2 hours, cooled in an ice bath, and extracted with EtOAc (2×400 mL). The combined extracts are washed with saturated brine, dried over sodium sulfate, filtered, and concentrated to a yellow solid (39 g, 97%). ESI/MS m/z 247.1 (M−H)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383642B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-0b6a76412b7d4af8ac7993cb8fbb8a5b |
| 出典メモ | uspto-grants-2013_02 |