참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetal | HCID 7765 | — |
| 반응물 | Ethyl 1-propenyl ether | HCID 13570 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 촉매 | Aluminum(III) Chloride | HCID 6451240 | — |
| 생성물 | 1,1,3-Triethoxy-2-methyl-butane | HCID 11830544 | 88% |
반응 단계
236 g of acetaldehyde diethyl acetal (abbreviation: acetal) and 1 g of aluminum chloride are added in 500 ml of four necked bottle under protection of nitrogen, the solution is freezed to −10° C., and kept at −10° C.˜−5° C., a mixture of 118 g of acetaldehyde diethyl acetal and 86 g (0.945 mol) of ethyl-(1-propenyl)-ether is slowly dropped, and continue to stir it for 10 min after finishing dropping, and the end of reaction is detected by GC. A saturated NaHCO3 solution is added in the reaction to neutralize it to pH=7, and to layer, the oil layer is dried by anhydrous sodium sulfate after being washed by water, and heated to 50° C.; most of acetaldehyde diethyl acetal is recycled, to obtain 169.6 g of 1,1,3-triethoxy-2-methyl-butane by vacuum distillation, and its content is 97.2%, and its yield is 88%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09187394B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_11 |
|---|
| ORD ID | ord-3ee62605852e49bfa7d087d4d683f11c |
|---|
| 출처 메모 | uspto-grants-2015_11 |
|---|