참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylene Glycol | HCID 174 | — |
| 반응물 | Trimethyl orthoformate | HCID 9005 | — |
| 반응물 | Diacetyl(methoxyimino)methane | HCID 536122 | — |
| 촉매 | p-Toluenesulfonic acid | HCID 6101 | — |
| 생성물 | (1E)-1-methoxyimino-1-(2-methyl-1,3-dioxolan-2-yl)propan-2-one | HCID 22967234 | 79.4% |
반응 단계
2400 g (39 mol) of ethylene glycol, 430 g (3.62 mol) of trimethyl orthoformate, 550 g (3.9 mol) of pentane-2,3,4-trione 3-(O-methyloxime) and 9 g of p-toluene sulfonic acid (46 mmol) were heated with stirring to 85° C. over a period of 15 min. After 30 min at 85° C., the mixture was cooled to room temperature. During the reaction, volatile components were distilled off via a column head. For work-up, the mixture was washed with saturated sodium bicarbonate solution and extracted with methyl tert-butyl ether, and the combined organic phases were washed twice with water and finally dried over magnesium sulfate. Distillative removal of the solvent gave 580 g of a red-brown oil (phys. data see Tab. 1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06441236B1 |
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| 출처 데이터셋 | uspto-grants-2002_08 |
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| ORD ID | ord-c53fe3edc8674c529c8e128872e6fe7a |
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| 출처 메모 | uspto-grants-2002_08 |
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