Triethylamine → 2-(4-Ethylphenyl)-4,4-dimethyl-2-oxazoline

HRID 480063

반응식

HRID 480063 반응식
[CH2:1]([C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=O)=[CH:5][CH:4]=1)[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH2:31][C:32]([CH3:36])([CH3:35])[CH2:33]O.C(N(CC)CC)C>C(#N)C.CCCCCC.C(OCC)(=O)C.ClC(Cl)(Cl)Cl>[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([C:7]2[O:9][CH2:33][C:32]([CH3:36])([CH3:35])[N:31]=2)=[CH:10][CH:11]=1)[CH3:2]

참가 물질

9

반응물 4

HCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 118072-Amino-2-methyl-1-propanolHCID 120864-Ethylbenzoic Acid

생성물 1

HCID 128725592-(4-Ethylphenyl)-4,4-dimethyl-2-oxazoline

시약·촉매·용매 4

HCID 5943Carbon Tetrachloride용매HCID 6342Acetonitrile용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-ethylbenzoic acid (3.80 g) in anhydrous acetonitrile (100 mL) was added under a nitrogen atmosphere, triphenylphosphine (20 g), 2-amino-2-methyl-1-propanol (2.74 mL) and triethylamine (28.2 mL). The mixture was cooled on an ice bath and then tetrachloromethane (5.36 mL) was added. The reaction mixture was allowed to stand at room temperature and stirred for 18 hours. To the reaction mixture was added ethyl acetate and hexane and the precipitate was removed by filtration. The concentration of the filtrate left a residue, which was purified by column chromatography on silica gel (hexane/ethyl acetate/=9/1/ to 6/1) to give the subject compound (1.15 g).

후처리

  1. temperatureThe mixture was cooled on an ice bath
  2. customto stand at room temperature
  3. customthe precipitate was removed by filtration
  4. waitThe concentration of the filtrate left a residue, which
  5. customwas purified by column chromatography on silica gel (hexane/ethyl acetate/=9/1/ to 6/1)

출처 및 근거

ORD 기록
ord-2e6c5084f567461f94019086ac8502ad
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649624B2

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