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Sodium Bicarbonate → N,N-dimethyl-N'-{5-[3-(1-methyl-1H-pyrazol-4-yl)-6-quinoxalinyl]-3-pyridinyl}sulfamide

HRID 734962
ノート
印刷プレビュー

反応式

HRID 734962 の反応式
Br[C:2]1[CH:11]=[C:10]2[C:5]([N:6]=[CH:7][C:8]([C:12]3[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=3)=[N:9]2)=[CH:4][CH:3]=1.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C([O-])(=O)C.[K+].Br[C:42]1[CH:43]=[C:44]([NH:48][S:49]([N:52]([CH3:54])[CH3:53])(=[O:51])=[O:50])[CH:45]=[N:46][CH:47]=1.C(=O)(O)[O-].[Na+]>O1CCOCC1.O.ClCCl.CCOCC>[CH3:53][N:52]([CH3:54])[S:49]([NH:48][C:44]1[CH:45]=[N:46][CH:47]=[C:42]([C:2]2[CH:11]=[C:10]3[C:5](=[CH:4][CH:3]=2)[N:6]=[CH:7][C:8]([C:12]2[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=2)=[N:9]3)[CH:43]=1)(=[O:50])=[O:51]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 516892Sodium BicarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 578432587-bromo-2-(1-methyl-1H-pyrazol-4-yl)quinoxalineHCID 57843357N'-(5-bromo-3-pyridinyl)-N,N-dimethylsulfamide

生成物 1

HCID 57843459
N,N-dimethyl-N'-{5-[3-(1-methyl-1H-pyrazol-4-yl)-6-quinoxalinyl]-3-pyridinyl}sulfamide
収率 57%

試薬・触媒・溶媒 4

HCID 6344Dichloromethane触媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

実験手順

In an oven dried high pressure vessel under a nitrogen atmosphere, 7-bromo-2-(1-methyl-1H-pyrazol-4-yl)quinoxaline (150 mg, 0.519 mmol), bis(pinacolato)diboron (158 mg, 0.623 mmol), potassium acetate (153 mg, 1.556 mmol), and 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex (18.98 mg, 0.026 mmol) in anhydrous 1,4-dioxane (2 mL) was stirred at 100° C. in an oil bath for 1 hr. The reaction mixture was cooled to room temperature. N′-(5-bromo-3-pyridinyl)-N,N-dimethylsulfamide (145 mg, 0.519 mmol) followed by sodium bicarbonate (131 mg, 1.556 mmol) in water (0.67 mL) were added to the reaction mixture and the vessel was sealed again. The reaction was stirred at 100° C. for 16.75 hours then cooled to room temperature. The reaction was filtered through Celite and the pad was washed with ethyl acetate. The bi-phasic mixture was separated in a separatory funnel. The organic layer was washed with brine (20 mL), dried over magnesium sulfate, and concentrated in vacuo to give a brown solid. Trituration of the brown solid in dichloromethane (3 drops) and ether (8 mL) provided the title compound (120 mg, 57%) as a light brown solid. MS(ES)+ m/e 410.2 [M+H]+.

後処理

  1. customIn an oven dried high pressure vessel under a nitrogen atmosphere
  2. additionwere added to the reaction mixture
  3. customthe vessel was sealed again
  4. temperaturethen cooled to room temperature
  5. filtrationThe reaction was filtered through Celite
  6. washthe pad was washed with ethyl acetate
  7. customThe bi-phasic mixture was separated in a separatory funnel
  8. washThe organic layer was washed with brine (20 mL)
  9. dry with materialdried over magnesium sulfate
  10. concentrationconcentrated in vacuo
  11. customto give a brown solid

出典と根拠

ORDレコード
ord-4bffdfd25a4b4573a17a28f3443ddd11
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592342B2

反応ノート

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