Thionyl Chloride → 4,4-Dimethyl-2-(4'-chloromethylbiphenyl-2-yl)oxazoline

HRID 1940938

반응식

HRID 1940938 반응식
[CH3:1][C:2]1([CH3:21])[CH2:6][O:5][C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]2[CH:18]=[CH:17][C:16]([CH2:19]O)=[CH:15][CH:14]=2)=[N:3]1.S(Cl)([Cl:24])=O.C(=O)([O-])O.[Na+]>C(Cl)Cl>[CH3:1][C:2]1([CH3:21])[CH2:6][O:5][C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]2[CH:18]=[CH:17][C:16]([CH2:19][Cl:24])=[CH:15][CH:14]=2)=[N:3]1

참가 물질

5

반응물 3

HCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 110658764,4-Dimethyl-2-(4'hydroxymethylbiphenyl-2-yl)oxazoline

생성물 1

HCID 109794774,4-Dimethyl-2-(4'-chloromethylbiphenyl-2-yl)oxazoline수율 98.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.0 g (3.55 mmol) of 4,4-dimethyl-2-(4'-hydroxymethylbiphenyl-2-yl)oxazoline was dissolved in methylene chloride (15 ml). Under cooling with ice. 0.51 g (4.29 mmol) of thionyl chloride was dropwise added thereto, followed by stirring for one hour. The reaction liquid was poured into an aqueous solution of sodium hydrogencarbonate, followed by the extraction with methylene chloride. After washing with water and drying, vacuum concentration was conducted. 1.05 g of the title compound was obtained as a crystal (yield 99%).

후처리

  1. temperatureUnder cooling with ice
  2. customThe reaction liquid
  3. extractionfollowed by the extraction with methylene chloride
  4. washAfter washing with water
  5. customdrying
  6. concentrationvacuum concentration

출처 및 근거

ORD 기록
ord-328be71ed94c4955b385d16c611a3962
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700938

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