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Dichloromethane → 3-[3-Chloro-4-(1-chloroethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole

HRID 551316
ノート
印刷プレビュー

反応式

HRID 551316 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:11]2[CH2:15][C:14]([C:20]3[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=3)([C:16]([F:19])([F:18])[F:17])[O:13][N:12]=2)[CH:5]=[CH:6][C:7]=1[CH:8](O)[CH3:9].[Cl:28]CCl>S(Cl)(Cl)=O.CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([C:11]2[CH2:15][C:14]([C:20]3[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=3)([C:16]([F:19])([F:18])[F:17])[O:13][N:12]=2)[CH:5]=[CH:6][C:7]=1[CH:8]([Cl:28])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6344DichloromethaneHCID 866315533-[3-Chloro-4-(1-hydroxyethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole

生成物 1

HCID 866315543-[3-Chloro-4-(1-chloroethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 24386Thionyl Chloride溶媒

実験手順

In a solution of 0.96 g of 3-[3-chloro-4-(1-hydroxyethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole in 20 mL of dichloromethane, 0.2 mL of thionyl chloride and a catalytic amount (2 to 3 drops) of N,N-dimethylformamide were added, and stirred at room temperature for 1 hour. After the completion of the reaction, the reaction mixture was poured into 20 mL of ice water, and the organic phase was collected, washed with water (20 mL×1) and then saturated sodium hydrogen carbonate aqueous solution (20 mL×3), and dehydrated with and dried over saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order, and then the solvent was distilled off under reduced pressure to obtain 0.88 g of the aimed product as yellow oily substance.

後処理

  1. customAfter the completion of the reaction
  2. customthe organic phase was collected
  3. washwashed with water (20 mL×1)
  4. dry with materialdried over saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-91ee259de6a3483eb0a1e3e0baa85a58
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07947715B2

反応ノート

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