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Hydrochloric Acid → 3-(4-methoxyphenyl)-7-phenyl-2-propyl-2H-indazole

HRID 1295043
ノート
印刷プレビュー

反応式

HRID 1295043 の反応式
Cl[C:2]1[C:10]2[C:6](=[C:7]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[N:8]([CH2:11][CH2:12][CH3:13])[N:9]=2)[CH:5]=[CH:4][CH:3]=1.Cl.[C:23]1([Mg]Br)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH3:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([C:7]2[N:8]([CH2:11][CH2:12][CH3:13])[N:9]=[C:10]3[C:6]=2[CH:5]=[CH:4][CH:3]=[C:2]3[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[CH:15][CH:16]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 688824767-chloro-3-(4-methoxyphenyl)-2-propyl-2H-indazoleHCID 178418255HCID 178418255、化合物

生成物 1

HCID 688851453-(4-methoxyphenyl)-7-phenyl-2-propyl-2H-indazole収率 78.8%

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 31275
1,4-Dioxane
溶媒

反応条件

温度
80 °C

実験手順

To a stirred solution of 7-Chloro-3-(4-methoxyphenyl)-2-propyl-2H-indazole (0.200 g, 0.66 mmol) in anhydrous dioxane (6 mL) was added tris(dibenzylideneacetone)-dipalladium(0) (0.0128 g, 0.013 mmol) and 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene.HCl (0.011 g, 0.07 mmol). Phenylmagnesium bromide (0.4 mL, 1.20 mmol, 3M in diethyl ether) was added and the reaction heated to 80° C. for 3 hours. After this time an additional equivalent of reagents was added and the reaction heated for an additional 18 hours. The reaction mixture was treated with 1N aqueous hydrochloric acid solution and extracted with ethyl acetate. The organic layer washed with water and saturated aqueous sodium chloride solution. After drying over anhydrous magnesium sulfate, the organic phase was filtered and the filtrate evaporated in vacuo to yield crude title compound. The oil was purified by silica gel column chromatography eluting with hexane/ethyl acetate (5/1) to provide the title compound as a white solid (0.178 g, 0.52 mmol, 78%).

後処理

  1. additionAfter this time an additional equivalent of reagents was added
  2. temperaturethe reaction heated for an additional 18 hours
  3. extractionextracted with ethyl acetate
  4. washThe organic layer washed with water and saturated aqueous sodium chloride solution
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. filtrationthe organic phase was filtered
  7. customthe filtrate evaporated in vacuo
  8. customto yield crude title compound
  9. customThe oil was purified by silica gel column chromatography
  10. washeluting with hexane/ethyl acetate (5/1)

出典と根拠

ORDレコード
ord-93eb66b16f0a427d879199118c6cdf07
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07241791B2

反応ノート

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