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ChemicalBook CAS DataBase List 5-BROMO-2,3-DIHYDRO-1H-PYRROLO[2,3-B]PYRIDINE
115170-40-6

5-BROMO-2,3-DIHYDRO-1H-PYRROLO[2,3-B]PYRIDINE synthesis

3synthesis methods
-

Yield:115170-40-6 95.6%

Reaction Conditions:

with hydrogen bromide;dihydrogen peroxide in dichloromethane at 25 - 30;Reagent/catalyst;

Steps:

3.2 (2) Synthesis of 5-bromo-7-azaporphyrin
a) 16.8g (0.14mol) of 7-azaporphyrin, 24.13g (0.143mol) of 48% hydrobromic acid, and 260g of methylene chloride were charged into a reaction flask and stirred uniformly to obtain a reaction mixture C;b) The reaction mixture temperature was controlled to 25 ~ 30 ° C, was added dropwise 20% of 20.20g of hydrogen peroxide to obtain a mixture D;c) mixture D is neutralized with a saturated aqueous solution of 60 g of sodium hydrogen sulfite until the red color in the reaction solution completely disappears, liquid separation, to obtain an organic phase E and an aqueous phase F;d) the organic phase E is washed with water, the amount of water is 200g;e) The organic phase E obtained in the step (d) recovers the dichloromethane solvent to obtain 26.6 g of 5-bromo-7-azaporphyrin product, the yield is 95.6%, and the product liquid chromatographic purity is ≥99%;

References:

Zhonggang Group Anshan Heat Energy Institute Co., Ltd.;Wang Haiyang;Wang Shoukai;Xu Zhe;Zhao Wei;Jiang Hui;Jin Dan;Xu Haoran CN107987076, 2018, A Location in patent:Paragraph 0048-0053; 0064-0069; 0074; 0080-0085

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