Potassium Phosphate, Tribasic → HCID 178489260、化合物

HRID 455954

反応式

HRID 455954 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH3:23])[C:14]3[C:13]([C:24]([CH3:27])([CH3:26])[CH3:25])=[N:12][NH:11][C:10]=3[C:9]2=[O:28])=[CH:4][CH:3]=1.[O:29]1[CH:33]=[CH:32][C:31](B(O)O)=[CH:30]1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C(C1C=C(C(C)C)C=C(C(C)C)C=1C1C=CC=CC=1P)(C)C>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].C(O)CCC>[C:24]([C:13]1[C:14]2[CH:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH3:23])[N:8]([C:5]3[CH:4]=[CH:3][C:2]([C:31]4[CH:32]=[CH:33][O:29][CH:30]=4)=[CH:7][CH:6]=3)[C:9](=[O:28])[C:10]=2[NH:11][N:12]=1)([CH3:25])([CH3:26])[CH3:27]

参加物

7

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 2734358Furan-3-boronic acidHCID 58067324(2',4',6'-Triisopropylbiphenyl-2-yl)phosphineHCID 178489255HCID 178489255、化合物

生成物 1

HCID 178489260HCID 178489260、化合物収率 63%

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 2631-Butanol溶媒

実験手順

To a mixture of 5-(4-bromophenyl)-3-t-butyl-4-(2-methoxyphenyl)-4,5-dihydro-1H-pyrrolo[3,4-c]pyrazol-6-one (0.10 g, 0.23 mmol), 3-furylboronic acid (0.038 g, 0.34 mmol), tripotassium phosphate (0.096 g, 0.45 mmol) and butanol (1 mL), (2′,4′,6′-tri-isopropylbiphenyl-2-yl)phosphine (0.009 g, 0.02 mmol) and tris(dibenzylideneacetone)dipalladium(0) (0.004 g, 0.004 mmol) were added under a nitrogen atmosphere, and the mixture was stirred under reflux for 3 hr. The reaction mixture was purified by silica gel column chromatography (ethyl acetate/n-hexane). The fraction was concentrated under reduced pressure and the precipitate was collected by filtration to give 3-t-butyl-5-(4-fur-3-ylphenyl)-4-(2-methoxyphenyl)-4,5-dihydro-1H-pyrrolo[3,4-c]pyrazol-6-one (0.061 g, 63%) as colorless crystals.

後処理

  1. additionwere added under a nitrogen atmosphere
  2. temperatureunder reflux for 3 hr
  3. customThe reaction mixture was purified by silica gel column chromatography (ethyl acetate/n-hexane)
  4. concentrationThe fraction was concentrated under reduced pressure
  5. filtrationthe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-d03777362e3946a3a0f3a4856ff4257b
出典データセット
uspto-grants-2013_07
特許番号
US08497263B2

関連ノート

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