Sulfuric acid magnesium salt (1:1) → 3-Bromothieno[2,3-b]pyridine

HRID 876784

反応式

HRID 876784 の反応式
[Br:1]Br.[S:3]1[C:7]2=[N:8][CH:9]=[CH:10][CH:11]=[C:6]2[CH:5]=[CH:4]1.P([O-])([O-])(O)=O.[K+].[K+].C(=O)(O)[O-].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)(Cl)Cl>[Br:1][C:5]1[C:6]2[C:7](=[N:8][CH:9]=[CH:10][CH:11]=2)[S:3][CH:4]=1

参加物

7

反応物 5

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 24408BromineHCID 24450Potassium Phosphate, DibasicHCID 289928Thieno(2,3-b)pyridineHCID 516892Sodium Bicarbonate

生成物 1

HCID 2899263-Bromothieno[2,3-b]pyridine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Bromine (2.08 g, 13 mmol) was dropwise added to a mixture of thieno[2,3-b]pyridine (J-2) (1.35 g, 10 mmol), dipotassium monohydrogen orthophosphate (940 mg, 5.4 mmol), sodium bicarbonate (840 mg 10 mmol), and magnesium sulfate (2.0 g, 16.7 mmol) in chloroform (40 mL) which has been stirred at reflux for 16 h, the resulting mixture was stirred under reflux for 24 h, then filtered and washed with DCM. The filtrate was concentrated, and purified by chromatography. MS (m/z): 214 (M+H)+.

後処理

  1. temperatureat reflux for 16 h
  2. stirringthe resulting mixture was stirred
  3. temperatureunder reflux for 24 h
  4. filtrationfiltered
  5. washwashed with DCM
  6. concentrationThe filtrate was concentrated
  7. custompurified by chromatography

出典と根拠

ORDレコード
ord-e6bddd748b86406bad8e56c13a380735
出典データセット
uspto-grants-2015_03
特許番号
US08987269B2

関連ノート

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