Sodium Carbonate → 5-Bromo-2-phenyl-4-(pyridin-4-yl)thiazole

HRID 538424

反応式

HRID 538424 の反応式
[C:1]1([C:7]2[S:8][CH:9]=[C:10]([C:12]3[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=3)[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])([O-])=O.[Na+].[Na+].[Br:24]Br>C(Cl)(Cl)Cl>[Br:24][C:9]1[S:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:11][C:10]=1[C:12]1[CH:13]=[CH:14][N:15]=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 10340Sodium Carbonate2 回HCID 24408Bromine2 回HCID 665911812-Phenyl-4-(pyridin-4-yl)thiazole

生成物 1

HCID 665905405-Bromo-2-phenyl-4-(pyridin-4-yl)thiazole

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To the solution of 2-phenyl-4-(pyridin-4-yl)thiazole (70 mg, 0.3 mmol) in CHCl3 was added Na2CO3 (311 mg, 2.9 mmol) and Br2 (75 μL, 1.470 mmol) at rt. After 1 h, additional charges of Na2CO3 (1 g, 9.4 mmol) and Br2 (0.5 mL, 1 mmol) were added and the reaction maintained for another hour. The reaction was diluted with CHCl3 and filtered through a pad of Celite, washing the filter cake thoroughly with CHCl3. The combined filtrates were concentrated of provide 0.5-bromo-2-phenyl-4-(pyridin-4-yl)thiazole which was carried forward without further purification: LCMS (m/z): 318.9 (MH+), tR=0.75 min.

後処理

  1. temperaturethe reaction maintained for another hour
  2. filtrationfiltered through a pad of Celite
  3. washwashing the filter cake thoroughly with CHCl3
  4. concentrationThe combined filtrates were concentrated
  5. customof provide 0
  6. custom5-bromo-2-phenyl-4-(pyridin-4-yl)thiazole which was carried forward without further purification

出典と根拠

ORDレコード
ord-8dcf3de9f7264282a6de8586de02af1c
出典データセット
uspto-grants-2014_10
特許番号
US08865732B2

関連ノート

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