참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Quinone | HCID 4650 | — |
| 반응물 | Boron trifluoride | HCID 6356 | — |
| 반응물 | Trimethyl orthoformate | HCID 9005 | — |
| 반응물 | 3-Butenoic acid, ion(1-) | HCID 6971089 | — |
| 생성물 | HCID 11159832 | HCID 11159832 | — |
반응 단계
A mixture of 56.00 g trimethyl ortho formate, 60.00 g vinylacetate, 0.75 g PdCl2(ACN)2, 0.60 g 1,4-benzoquinone, and 1.00 ml BF3*OEt2 was stirred at 30° C., and low boiling impurities were removed from the reaction mixture through the application of a slight vacuum. A fractionation column was installed to prevent losses of starting materials and/or products. After 2.3 hours, the ratio of 1,1,3,3-tetramethoxypropane to 1-acetoxy-1,3,3-trimethoxypropane, and the isomeric 1,3-diacetoxy-1,3-dimethoxy-propanes was determined by CG-analysis to be 1.0:2.4:1.3 on the basis of the FID-area-percentages. In a comparative experiment, without removal of low boiling impurities, the referring ratio was determined to be 1.0:1.48:0.50. Both reaction mixtures still contained an excess of vinylacetate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06355844B1 |
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| 출처 데이터셋 | uspto-grants-2002_03 |
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| ORD ID | ord-96361f58c4244f7cb626f288b6f32d34 |
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| 출처 메모 | uspto-grants-2002_03 |
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