N-[3-Fluoro-4-[(methylamino)carbonyl]phenyl]-2-methylalanine synthesis
- Product Name:N-[3-Fluoro-4-[(methylamino)carbonyl]phenyl]-2-methylalanine
- CAS Number:1289942-66-0
- Molecular formula:C12H15FN2O3
- Molecular Weight:254.26
749927-69-3
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1289942-66-0
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Yield:1289942-66-0 88.7%
Reaction Conditions:
with 2-acetylcyclohexanone;potassium carbonate;copper(l) chloride in N,N-dimethyl-formamide at 110; for 16 h;
Steps:
1 Example 1: Synthesis of 2- (3-fluoro-4- (methylcarbamoyl) phenylamino) -2-methylpropanoic acid
N-methyl-4-bromo-2-fluoro-benzamide (A) (600 g, 2.6 mol, 1.0 eq), 2-amino-2-methylpropionic acid (400 g, 3.9 mol, 1.5 eq) Potassium carbonate (893g, 6.5mol, 2.5eq), CuCl (51g, 0.52mol, 0.2eq), add to DMF (3600ml), stir well, add 2-acetylcyclohexanone (73g, 0.52mol, 0.2eq) ), Reaction at 110 ° C for 16 hours under inert gas. After the reaction was completed, the reaction solution was cooled to room temperature, purified water and ethyl acetate were added and extracted twice, and the organic layers were combined. The organic layer was adjusted to be acidic with a 1N hydrochloric acid solution, crystallized by stirring at 0-5 ° C, filtered, the filter cake was washed with purified water, and dried at 60 ° C to obtain 583 g of a yellow solid with a yield of 88.7%.
References:
CN110872258,2020,A Location in patent:Paragraph 0015
749927-69-3
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1289942-66-0
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1289942-66-0
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2052-01-9
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1289942-66-0
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1289942-66-0
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