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Dimethyl Sulfoxide → 7-(2-{2-[3-Fluoro-5-(trifluoromethyl)phenyl] (1,3-oxazol-5-yl)}ethoxy)-3-(4-hydroxyphenyl)chromen-4-one

HRID 1694656
ノート
印刷プレビュー

反応式

HRID 1694656 の反応式
[OH:1][C:2]1[CH:19]=[CH:18][C:5]([C:6]2[C:15](=[O:16])[C:14]3[C:9](=[CH:10][C:11]([OH:17])=[CH:12][CH:13]=3)[O:8][CH:7]=2)=[CH:4][CH:3]=1.[F:20][C:21]1[CH:22]=[C:23]([C:36]([F:39])([F:38])[F:37])[CH:24]=[C:25]([C:27]2OC=[C:30]([CH2:32][CH2:33][CH2:34]I)[N:31]=2)[CH:26]=1.C(=O)([O-])[O-].[Cs+].[Cs+].CS(C)=O.[OH2:50]>>[F:20][C:21]1[CH:26]=[C:25]([C:27]2[O:50][C:32]([CH2:33][CH2:34][O:17][C:11]3[CH:10]=[C:9]4[C:14]([C:15](=[O:16])[C:6]([C:5]5[CH:18]=[CH:19][C:2]([OH:1])=[CH:3][CH:4]=5)=[CH:7][O:8]4)=[CH:13][CH:12]=3)=[CH:30][N:31]=2)[CH:24]=[C:23]([C:36]([F:38])([F:39])[F:37])[CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 679Dimethyl SulfoxideHCID 962WaterHCID 10796Cesium carbonateHCID 5281708DaidzeinHCID 672790242-[5-Fluoro-3-(trifluoromethyl)phenyl]-4-(3-iodopropyl)-1,3-oxazole

生成物 1

HCID 249606237-(2-{2-[3-Fluoro-5-(trifluoromethyl)phenyl] (1,3-oxazol-5-yl)}ethoxy)-3-(4-hydroxyphenyl)chromen-4-one
収率 76%

実験手順

4′,7-Dihydroxyisoflavone (31.3 mg, 0.123 mmol), 2-[5-fluoro-3-(trifluoromethyl)phenyl]-4-(3-iodopropyl)-1,3-oxazole (48.9 mg, 0.123 mmol, 1.0 equiv.) and cesium carbonate (40.0 mg, 0.123 mmol, 1.0 equiv) were placed in a 25 mL flask. To the flask was added dimethylsulfoxide (3 mL) at room temperature to dissolve the starting materials, and the reaction mixture stirred room temperature for 15 hours. To the mixture were added water (30 mL) and the whole was extracted with ethyl acetate (30 mL×3). The combined organic layers were washed with brine (30 mL) and dried with sodium sulfate to give a crude mixture as colorless oil (64.2 mg). The crude mixture was purified by column-chromatography (SiO2=80 g, hexane/EtOAc=2:1 to 1:1) to give 7-(2-{2-[3-fluoro-5-(trifluoromethyl)phenyl](1,3-oxazol-5-yl)}ethoxy)-3-(4-hydroxyphenyl)chromen-4-one (49.1 mg, 0.0934 mmol, 76%) as colorless crystals. Similarly prepared was 7-(3-{2-[3-fluoro-5-(trifluoromethyl)phenyl](1,3-oxazol-4-yl)}propoxy)-3-(4-hydroxyphenyl)chromen-4-one.

後処理

  1. dissolutionto dissolve the starting materials
  2. extractionthe whole was extracted with ethyl acetate (30 mL×3)
  3. washThe combined organic layers were washed with brine (30 mL)
  4. dry with materialdried with sodium sulfate
  5. customto give a crude mixture as colorless oil (64.2 mg)
  6. customThe crude mixture was purified by column-chromatography (SiO2=80 g, hexane/EtOAc=2:1 to 1:1)

出典と根拠

ORDレコード
ord-d981441b39e34f67868eccb043a1931c
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158810B2

反応ノート

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