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ChemicalBook CAS DataBase List 2-Amino-3-benzyloxypyridine

2-Amino-3-benzyloxypyridine synthesis

3synthesis methods
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Yield:24016-03-3 77.3%

Reaction Conditions:

with tetrabutylammomium bromide;sodium hydroxide in water at 40 - 75; for 6 h;Large scale;

Steps:

1 Example 1: Intermediate II: Preparation of 2-amino-3-benzyloxypyridine
temperature below 40 ° C, to the 300L stainless steel reactor 48L of purified water was added slowly stirring 48kg sodium hydroxide, stirring until dissolved.To sodium hydroxide solution followed by adding 16kg 2-amino-3-hydroxypyridine, 1.6kg tetrabutylammonium bromide, 17.92L benzyl chloride, plus warming to 70 ~ 75 ° C reaction 6 hours, stirring was stopped,Let stand, liquid separation; aqueous phase extraction with toluene (20Lx3);Purified water washing (30Lx2), the organic phase was collected, concentrated to a large amount of solid precipitation, temperature 0 ~ 5 ° C, crystallization was stirred for 2 hours, centrifuged,The filter cake was rinsed with 3.2 L of pre-cooled toluene and dried under vacuum at 50~55 ° C. for 3 hours to afford Intermediate II as a bright yellow solid, 22.5 kg of 2-amino-3-benzyloxypyridine, with a molar yield of 77.3% , Purity 99.53%.

References:

Jinan Cornwall, Ontario Pharmaceutical Technology Co., Ltd.;Zhang Dongmei;Zhang Ying;Xu Jiaping;Ai Leifeng;Zheng Liangwen;Sun Limeng CN107311998, 2017, A Location in patent:Paragraph 0035-0036

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