Tyramine → 4-Vinylacetamidoethyl phenol

HRID 1294397

반응식

HRID 1294397 반응식
[NH2:1][CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.C(N(CC)CC)C.[CH:18]([CH2:20][C:21](Cl)=[O:22])=[CH2:19]>C(Cl)Cl>[CH:18]([CH2:20][C:21]([NH:1][CH2:2][CH2:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)=[O:22])=[CH2:19]

참가 물질

5

반응물 3

HCID 5610TyramineHCID 8471TriethylamineHCID 10975427But-3-enoyl Chloride

생성물 1

HCID 626796864-Vinylacetamidoethyl phenol수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A 1000-mL 3-neck, round bottom flask connected with a reflux condenser and a drying tube, is charged with 250 mL of methylene chloride, 5.48 grams (0.04 mole) 4-aminoethylphenol and 4.04 grams (0.04 mole) triethylamine. The contents are chilled with an ice bath. Through a dropping funnel, 4.18 g (0.04 mole) of vinylacetyl chloride is added into the flask over a period of 30 minutes. The ice bath is then removed and the contents are continuously stirred overnight. The mixture is then filtered and then condensed using a rotavapor. High performance liquid chromatography (HPLC) analysis indicates only one major product. The product is then passed through silica gel chromatography to give a final purified product with a yield of at least 80 percent. The product is identified by NMR and Mass Spectroscopy.

후처리

  1. customA 1000-mL 3-neck, round bottom flask connected with a reflux condenser and a drying tube
  2. temperatureThe contents are chilled with an ice bath
  3. customThe ice bath is then removed
  4. filtrationThe mixture is then filtered
  5. customcondensed
  6. customto give
  7. customa final purified product with a yield of at least 80 percent

출처 및 근거

ORD 기록
ord-32ffaa4cb2b34f4482811eb634154002
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07241312B2

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