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

HRID 714003

反応式

HRID 714003 の反応式
[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]

参加物

5

反応物 3

HCID 7765Acetal2 回HCID 13570Ethyl 1-propenyl etherHCID 516892Sodium Bicarbonate

生成物 1

HCID 118305441,1,3-Triethoxy-2-methyl-butane収率 88%

試薬・触媒・溶媒 1

HCID 6451240Aluminum(III) Chloride触媒

反応条件

温度
50 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-3ee62605852e49bfa7d087d4d683f11c
出典データセット
uspto-grants-2015_11
特許番号
US09187394B2

関連ノート

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