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Sodium Carbonate → [1,1'-Biphenyl]-4-sulfonamide, N-(4-hydroxybutyl)-4'-(trifluoromethyl)-

HRID 2425137
ノート
印刷プレビュー

反応式

HRID 2425137 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][NH:6][S:7]([C:10]1[CH:15]=[CH:14][C:13](Br)=[CH:12][CH:11]=1)(=[O:9])=[O:8].[F:17][C:18]([F:29])([F:28])[C:19]1[CH:24]=[CH:23][C:22](B(O)O)=[CH:21][CH:20]=1.C([O-])([O-])=O.[Na+].[Na+]>C(O)C.C1(C)C=CC=CC=1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][NH:6][S:7]([C:10]1[CH:15]=[CH:14][C:13]([C:22]2[CH:23]=[CH:24][C:19]([C:18]([F:29])([F:28])[F:17])=[CH:20][CH:21]=2)=[CH:12][CH:11]=1)(=[O:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 27343894-(Trifluoromethyl)phenylboronic acidHCID 160947204-Bromo-N-(4-hydroxybutyl)benzene-1-sulfonamide

生成物 1

HCID 11682252[1,1'-Biphenyl]-4-sulfonamide, N-(4-hydroxybutyl)-4'-(trifluoromethyl)-

試薬・触媒・溶媒 3

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒
HCID 702Ethanol溶媒
HCID 1140Toluene溶媒

実験手順

4-Bromophenyl-sulfonic acid-(4-hydroxybutyl)-amide (1 g) was dissolved in ethanol (8 mL) and toluene (8 mL). 4-Trifluoromethylphenyl boronic acid (1 g) was added, followed by 2 M Na2CO3 (8 mL). Tetrakis(triphenylphosphine) palladium (0.25 g) was added and the mixture heated to reflux under nitrogen for 3 hours with vigorous stirring. The organic solvents were evaporated and the residue dissolved in ethyl acetate (100 mL) and washed with water (100 mL) then saturated NaCl solution (100 mL). The organic phase was dried (Na2SO4), evaporated and the residue purified by column chromatography (ethyl acetate/petrol) to give the title compound as a white solid. δC (DMSO, 62.9 MHz): 25.9, 29.6, 42.6, 60.2, indistinct m, 140.4, 142.2 and 142.6. δH (DMSO, 250 MHz): 1.41 (4H, m), 2.77 (2H, m), 3.33 (2H, m), 4.39 (1H, t, NH), 7.83-7.94 (6 H, m) and 7.96 (2H, d, J 8.5).

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux under nitrogen for 3 hours with vigorous stirring
  3. customThe organic solvents were evaporated
  4. dissolutionthe residue dissolved in ethyl acetate (100 mL)
  5. washwashed with water (100 mL)
  6. dry with materialThe organic phase was dried (Na2SO4)
  7. customevaporated
  8. customthe residue purified by column chromatography (ethyl acetate/petrol)

出典と根拠

ORDレコード
ord-98d38c81eaae43b1b7b712a4538acfe8
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07964643B2

反応ノート

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