5-broMo-N,3-diMethylpyridin-2-aMine synthesis
- Product Name:5-broMo-N,3-diMethylpyridin-2-aMine
- CAS Number:245765-66-6
- Molecular formula:C7H9BrN2
- Molecular Weight:201.06
123-39-7
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3430-18-0
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245765-66-6
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Yield: 84.2%
Reaction Conditions:
with sodium hydride in N,N-dimethyl-formamide at 100; for 3 h;Temperature;Reagent/catalyst;
Steps:
1.3; 2.3; 3.3; 4.3 (3) Preparation of (5-bromo-3-methyl-pyridin-2-yl) -methylamine
Add 125 g of DMF to a 1 L four-necked flask, lower the temperature to 10 ° C, add 5.1 g (0.21 mol) of sodium hydride, stir to dissolve,Add 12.4 g (0.21 mol) of N-methylformamide and 50.2 g (0.2 mol) of 2,5-dibromo-3-methylpyridine, raise the temperature to 100 ° C, and hold the reaction for 3 hours.Reduce the temperature to 20-40 , add 250g of water, adjust the pH to 1,130g with 30% hydrochloric acid to extract impurities, separate the lower aqueous layer, and adjust the pH of the aqueous layer to 9.5-10.5 with 30% liquid alkali.Extract with 200 g of isopropyl acetate, wash the upper organic layer with 0.5% dilute hydrochloric acid to pH 7-8, remove the lower aqueous layer, and distill the isopropyl acetate to dryness under reduced pressure.Distill isopropyl acetate under reduced pressure at a temperature of 45-50 ° C and a degree of vacuum of -0.1 to -0.09 MPa; add 120 g of n-hexane to reduce the temperature to 0-10 ° C and crystallize to obtain flaky crystals.After drying at 80 ° C, 33.8 g of (5-bromo-3-methyl-pyridin-2-yl) -methylamine was obtained with a yield of 84.2% and an HPLC content of 99.7%.The benzoic acid content was not detected, and the N- (3-bromo-5-methylpyridin-2yl) -N-methylbenzamide was 0.05%, and the remaining single impurities were less than 0.2%.
References:
Changzhou Qihui Pharmaceutical Co., Ltd.;Inner Mongolia Qihui Chemical Co., Ltd.;Lianyungang Yahui Pharmaceutical And Chemical Co., Ltd.;Zhu Jianmin;Su Wenjie;Wang Xuecheng CN110563643, 2019, A Location in patent:Page/Page column 6-9
3430-21-5
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74-88-4
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245765-66-6
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29241-60-9
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245765-66-6
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1603-40-3
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245765-66-6
83 suppliers
$45.00/50mg