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

HRID 850822

반응식

HRID 850822 반응식
[CH2:1]([O:3][CH:4]([O:6][CH2:7][CH3:8])[CH3:5])[CH3:2].[CH:9]([O:12][CH2:13][CH3:14])=[CH:10]C.[C:15](=O)([O-])[O-].[Na+].[Na+]>B(F)(F)F.CCOCC>[CH2:1]([O:3][CH:4]([O:6][CH2:7][CH3:8])[CH:5]([CH3:15])[CH:9]([O:12][CH2:13][CH3:14])[CH3:10])[CH3:2]

참가 물질

5

반응물 3

HCID 7765AcetalHCID 10340Sodium CarbonateHCID 13570Ethyl 1-propenyl ether

생성물 1

HCID 118305441,1,3-Triethoxy-2-methyl-butane수율 66.2%

시약·촉매·용매 1

HCID 8000Boron trifluoride etherate촉매

반응 조건

온도
35 °C

실험 절차

900 g (7.4 mol) of acetaldehyde diethyl acetal (purity according to GC: 97%) and 0.85 g (0.75 ml, 6 mmol, 0.25 mol %) of boron trifluoride etherate were placed in a 2 l two-necked round flask fitted with a magnetic stirrer, a thermometer and a dropping funnel. 220 g (2.5 mol) of ethyl (1-propenyl) ether were added dropwise within about 30 minutes while cooling occasionally with ice at a temperature of about 35° C., but a maximum of 40° C. After completion of the addition the mixture was stirred at room temperature for a further 30 minutes. Then, 4 g of solid, powdered sodium carbonate were added thereto and the mixture was stirred at room temperature for 2.5 hours. Then the mixture was suction filtered and the excess acetaldehyde diethyl acetal was distilled off on a Raschig column, (30×2.5 cm) at 100 mbar. About 1 l of acetaldehyde diethyl acetal (content according to GC. 91%) was recovered in this manner at a boiling point of 40-43° C. The residue was then fractionated on the same column at a pressure of 12-13 mbar. This gave 344.5 g (66.2% yield) of 1,1,3-triethoxy-2-methyl-butane as a water-clear liquid with a boiling point of 81-84° C. and a content of 98.2% according to GC.

후처리

  1. customfitted with a magnetic stirrer
  2. customa maximum of 40° C
  3. additionAfter completion of the addition the mixture
  4. stirringthe mixture was stirred at room temperature for 2.5 hours
  5. filtrationfiltered
  6. distillationthe excess acetaldehyde diethyl acetal was distilled off on a Raschig column, (30×2.5 cm) at 100 mbar
  7. customAbout 1 l of acetaldehyde diethyl acetal (content according to GC. 91%) was recovered in this manner at a boiling point of 40-43° C

출처 및 근거

ORD 기록
ord-86926ac3b49043d8b2d50fb33a237c4a
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06018075

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