Acetal → 1,1,3-Triethoxy-2-methyl-butane

HRID 714003

반응식

HRID 714003 반응식
[CH2:1]([O:3][CH:4]([O:6][CH2:7][CH3:8])[CH3:5])[CH3:2].[CH2:9]([O:11][CH:12]=[CH:13]C)[CH3:10].[C:15]([O-])(O)=O.[Na+]>[Cl-].[Al+3].[Cl-].[Cl-]>[CH2:1]([O:3][CH:4]([O:6][CH2:7][CH3:8])[CH:5]([CH3:15])[CH:9]([O:11][CH2:12][CH3:13])[CH3:10])[CH3:2]

참가 물질

5

반응물 3

HCID 7765Acetal2회HCID 13570Ethyl 1-propenyl etherHCID 516892Sodium Bicarbonate

생성물 1

HCID 118305441,1,3-Triethoxy-2-methyl-butane수율 88%

시약·촉매·용매 1

HCID 6451240Aluminum(III) Chloride촉매

반응 조건

온도
50 °C

실험 절차

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%.

후처리

  1. customis freezed to −10° C.
  2. customkept at −10° C.˜−5° C.
  3. additionis slowly dropped
  4. customthe end of reaction
  5. dry with materialto layer, the oil layer is dried by anhydrous sodium sulfate
  6. washafter being washed by water

출처 및 근거

ORD 기록
ord-3ee62605852e49bfa7d087d4d683f11c
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187394B2

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