참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | O-Xylene | HCID 7237 | — |
| 반응물 | Dimethyl Carbonate | HCID 12021 | — |
| 반응물 | Cyclohexylacetone | HCID 66899 | — |
| 반응물 | Potassium methoxide | HCID 23664618 | — |
| 용매 | Acetic acid--water (1/1) | HCID 21899381 | — |
| 생성물 | Methyl beta-oxocyclohexanebutanoate | HCID 539146 | 72.8% |
반응 단계
A 500 ml flask was charged with 120 g xylene, 33.8 g of solid potassium methylate (3.2 molar equivalent) and 34.0 g of dimethylcarbonate (2.5 molar equivalent). The slurry was heated to 50° C. and over the course of 4 hours 24.2 g of 1-cyclohexylpropan-2-one (87% GC, 1 molar equivalent) was added. Stirring was continued for 2 hours and then the reaction mixture was cooled to 25° C. 95 g of an acetic acid/water mixture (1:2) was then added carefully. After decantation the aqueous phase was drained and the organic phase concentrated. The crude product was distilled leading to 24.9 g of methyl 4-cyclohexyl-3-oxobutanoate (81% GC, 68% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08841488B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-364daa418f5d4b908e74f037082ee828 |
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| 출처 메모 | uspto-grants-2014_09 |
|---|
