Tyramine → 4-Vinylacetamidoethyl phenol

HRID 1294397

反応式

HRID 1294397 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 626796864-Vinylacetamidoethyl phenol収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-32ffaa4cb2b34f4482811eb634154002
出典データセット
uspto-grants-2007_07
特許番号
US07241312B2

関連ノート

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