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Butyl vinyl ether → N-Methyl-N-phenylprop-2-enamide

HRID 9933
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HRID 9933 반응식
[CH3:1][N:2]([CH:9]=[O:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH:11](OCCCC)=[CH2:12].ClC(OC(=O)OC(Cl)(Cl)Cl)(Cl)Cl>O1CCOCC1>[CH3:1][N:2]([C:9]([CH:11]=[CH2:12])=[O:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8108Butyl vinyl etherHCID 66737N-MethylformanilideHCID 94429Triphosgene

생성물 1

HCID 234887N-Methyl-N-phenylprop-2-enamide수율 70.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of N-methylformanilide (30 g), butyl vinyl ether (22.2 g) in 25 ml of 1,4-dioxane under stirring at 10–15° C., a solution of bis-trichloromethylcarbonate (28.3 g) in 50 ml of 1,4-dioxane is added dropwise in 90 min. The reaction mixture is kept under stirring at room temperature overnight, then the solvent is evaporated under reduced pressure. Tert-butyl methyl ether (75 ml) and water (55 ml) are added, the mixture is cooled at about 5–10° C. and the pH is corrected to about 7 by adding sodium hydroxide 30% aqueous solution (55 g). After separation of the phases, the aqueous layer is extracted with tert-butyl methyl ether (70 ml) and the combined organic layers are evaporated under reduced pressure. To the residue tert-butyl methyl ether (50 ml) is added and the mixture is cooled at −15° C. for 90 minutes. The precipitate is filtered on Buchner, washed twice with tert-butyl methyl ether (25 ml×2) and dried at room temperature under vacuum overnight. 25.21 g of pure compound are obtained (70% molar yield)

후처리

  1. customthe solvent is evaporated under reduced pressure
  2. additionTert-butyl methyl ether (75 ml) and water (55 ml) are added
  3. temperaturethe mixture is cooled at about 5–10° C.
  4. additionby adding sodium hydroxide 30% aqueous solution (55 g)
  5. customAfter separation of the phases
  6. extractionthe aqueous layer is extracted with tert-butyl methyl ether (70 ml)
  7. customthe combined organic layers are evaporated under reduced pressure
  8. additionTo the residue tert-butyl methyl ether (50 ml) is added
  9. temperaturethe mixture is cooled at −15° C. for 90 minutes
  10. filtrationThe precipitate is filtered on Buchner
  11. washwashed twice with tert-butyl methyl ether (25 ml×2)
  12. customdried at room temperature under vacuum overnight

출처 및 근거

ORD 기록
ord-96aef0fe07034eea9b0b57368813915a
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091382B2

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