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ChemicalBook CAS DataBase List N-[3-Fluoro-4-[(methylamino)carbonyl]phenyl]-2-methylalanine
1289942-66-0

N-[3-Fluoro-4-[(methylamino)carbonyl]phenyl]-2-methylalanine synthesis

9synthesis methods
-

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 Synthesis
4-Bromo-2-fluoro-N-methylbenzamide

749927-69-3
286 suppliers
$40.00/1g

15028-41-8 Synthesis
ALPHA-AMINOISOBUTYRIC ACID METHYL ESTER HYDROCHLORIDE

15028-41-8
207 suppliers
$9.00/10g

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