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Potassium Carbonate → 3-Hydroxy-2,2-dimethylpropyl 2,2,4-trimethyl-3-oxopentanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,2,4,4-Tetramethyl-1,3-cyclobutanedione | HCID 13617 | — |
| 反応物 | Neopentyl glycol | HCID 31344 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Hydroxy-2,2-dimethylpropyl 2,2,4-trimethyl-3-oxopentanoate | HCID 86667140 | 100% |
反応手順
To a 1-liter round bottom flask was charged 2,2,4,4-tetramethyl-1,3-cyclobutanedione (140.2 g, 1.0 moles), neopentyl glycol (208.3 g, 2.0 moles), potassium carbonate (138 g, 1.0 moles) and 500 grams methylene chloride. The batch was heated to reflux for 3 hours then cooled and clarified to remove salts. Methylene chloride was removed with a rotary evaporator and 250 grams of toluene added. The organic layer was washed with 6×50 mL of demineralized water and dried with anhydrous sodium sulfate. Toluene was removed at 3 mmHg and 75° C. to provide 244.4 g of product. GC assay of the product was 96.2%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029451B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-5cca6038af9142acab008566e836fa34 |
| 出典メモ | uspto-grants-2015_05 |