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Toluene → HCID 54102009, 화합물

HRID 573494
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HRID 573494 반응식
[PH4+].[C:2]1([CH3:8])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9](=[O:12])([O-])[O-:10].[K+].[K+].[CH:15](=O)/[CH:16]=C/C>O>[C:9]([O:10][CH2:15][CH3:16])(=[O:12])[CH2:3][CH2:4][CH:5]=[CH:6][CH:7]=[CH:2][CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 447466CrotonaldehydeHCID 5460504Phosphonium

생성물 1

HCID 54102009HCID 54102009, 화합물수율 74%

시약·촉매·용매 1

HCID 962Water용매

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온도
65 °C

실험 절차

Next, in a stream of nitrogen, the phosphonium salt (b) (420 g, 0.92 mol), toluene (1600 ml), potassium carbonate (506.2 g, 3.66 mol), and crotonaldehyde (256.7 g, 3.66 mol) were put into a 5-L flask, followed by stirring at 65° C. for 7 hours. The reaction solution was cooled to room temperature, and water (840 g) was put thereinto, followed by stirring for 30 minutes, and then subjected to separation of liquid. The solvent was evaporated from the organic layer under a reduced pressure. A solid thus precipitated was removed by filtration. This solution was distilled under a reduced pressure (65 to 70° C./1.5 torr), and ethyl 4,6-octadienoate (c) was obtained (114.4 g, yield 74%).

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. stirringby stirring for 30 minutes
  3. customsubjected to separation of liquid
  4. customThe solvent was evaporated from the organic layer under a reduced pressure
  5. customA solid thus precipitated
  6. customwas removed by filtration
  7. distillationThis solution was distilled under a reduced pressure (65 to 70° C./1.5 torr)

출처 및 근거

ORD 기록
ord-d2309b1d195b4e4ea8b719d5727d0844
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09029593B2

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