2-nitro-N-(5-chloro-pyridin-2-yl)-5-methoxy-benzamide synthesis
- Product Name:2-nitro-N-(5-chloro-pyridin-2-yl)-5-methoxy-benzamide
- CAS Number:280773-16-2
- Molecular formula:C13H10ClN3O4
- Molecular Weight:307.69
Yield:280773-16-2 96.2%
Reaction Conditions:
with 1-hydroxy-pyrrolidine-2,5-dione;1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride in tetrahydrofuran at 20; for 1 h;Solvent;Temperature;
Steps:
4 Example 4
19.7 g (0.1 mol) of 5-methoxy-2-nitrobenzoic acid, 13.8 g (0.12 mol) of N-hydroxysuccinimide and18.6 g (0.12 mol) of EDC was added to a three-necked flask, 157.6 ml of tetrahydrofuran was added to dissolve the mixture, and the reaction was stirred at 20° C. for 1 hour. 12.8 g (0.1 mol) of 2-amino-5-chloropyridine was added to continue the reaction.TLC detection reaction is completed, the reaction solution was cooled to 5 ° C, the reaction solution was added 1260 ml of water and stirred for 7 hours, filtered, cake was washed with 40 ml of water, followed by 40 ml of ethanol.The filter cake was vacuum dried at 40° C. for 10 hours to give 29.6 g.Yield 96.2%, HPLC detection 99.6%.
References:
CN107778224,2018,A Location in patent:Paragraph 0026-0027; 0028-0029; 0030-0031; 0032-0033
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