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Sodium Carbonate → HCID 178489286、化合物

HRID 384312
ノート
印刷プレビュー

反応式

HRID 384312 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8]2[NH:12][N:11]=[N:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[CH3:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]2[NH:12][N:11]=[N:10][N:9]=2)[CH:3]=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 3

HCID 10340Sodium CarbonateHCID 27339582-Methoxyphenylboronic acidHCID 178419385HCID 178419385、化合物

生成物 1

HCID 178489286HCID 178489286、化合物収率 68.2%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 31275
1,4-Dioxane
溶媒

実験手順

5-(3-Bromo-phenyl)-1H-tetrazole 8b (20 g, 89 mmol) and 2-methoxybenzeneboronic acid (14.2 g, 93.3 mmol) were dissolved in 530 mL of 1,4-dioxane followed by addition of tetrakis(triphenylphosphine)palladium (1.84 g) and sodium carbonate (18.9 g, 178 mmol) under argon atmosphere. The reaction mixture was heated to reflux overnight. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure to remove 1,4-dioxane and then hydrochloric acid (200 mL, 6 mol/L) was added. The mixture was cooled for 2 hours and the layers were separated. The organic layer was collected and concentrated. The residue was dissolved in 500 mL of ethyl acetate and washed with 250 mL of water. The mixture was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was dissolved in 25 mL of ethyl acetate and standing overnight. The mixture was filtered to obtain the title compound 5-(2′-methoxy-biphenyl-3-yl)-1H-tetrazole 8c (15 g, yield 68.2%) as a light yellow solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux overnight
  3. concentrationThe mixture was concentrated under reduced pressure
  4. customto remove 1,4-dioxane
  5. additionhydrochloric acid (200 mL, 6 mol/L) was added
  6. temperatureThe mixture was cooled for 2 hours
  7. customthe layers were separated
  8. customThe organic layer was collected
  9. concentrationconcentrated
  10. dissolutionThe residue was dissolved in 500 mL of ethyl acetate
  11. washwashed with 250 mL of water
  12. dry with materialThe mixture was dried over anhydrous sodium sulfate
  13. concentrationconcentrated under reduced pressure
  14. dissolutionThe residue was dissolved in 25 mL of ethyl acetate
  15. filtrationThe mixture was filtered

出典と根拠

ORDレコード
ord-0a1f51286c28439397ea96f91c98082b
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367710B2

反応ノート

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