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

HRID 9935
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HRID 9935 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-enamide

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. Toluene (50 ml) and water (200 ml) are added, the mixture is cooled at about 5–10° C. and the pH is corrected to about 7 by adding sodium hydroxide 15% aqueous solution (30 ml). After separation of the phases, the aqueous layer is extracted twice with toluene (50 ml×2) and the combined organic layers are washed with water (50 ml) and evaporated under reduced pressure. The obtained residue (32.3 g, containing, according to HPLC assay, 28.7 g of pure product, 81% molar yield) is used for the next step of the synthesis without any further purification.

후처리

  1. customthe solvent is evaporated under reduced pressure
  2. additionToluene (50 ml) and water (200 ml) are added
  3. temperaturethe mixture is cooled at about 5–10° C.
  4. additionby adding sodium hydroxide 15% aqueous solution (30 ml)
  5. customAfter separation of the phases
  6. extractionthe aqueous layer is extracted twice with toluene (50 ml×2)
  7. washthe combined organic layers are washed with water (50 ml)
  8. customevaporated under reduced pressure
  9. additionThe obtained residue (32.3 g, containing, according to HPLC assay, 28.7 g of pure product, 81% molar yield)
  10. customis used for the next step of the synthesis without any further purification

출처 및 근거

ORD 기록
ord-de574b356eba403c974162d6944dc7cc
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091382B2

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