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

HRID 743754ノート

反応式

HRID 743754 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%). m.p.; 72°-75° C.

後処理

  1. additionwas dropwise added
  2. customThe reaction liquid
  3. extractionfollowed by the extraction with methylene chloride
  4. washAfter washing with water
  5. customdrying
  6. concentrationvacuum concentration

出典と根拠

ORDレコード
ord-01bb6305206246fd99672bfa1b49aa91
出典データセット
uspto-grants-1996_09
特許番号
US05557002

反応ノート

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