1-Fluoro-cyclopropanecarboxylic acid synthesis

Yield:137081-41-5 38%

Reaction Conditions:

with triethylamine tris(hydrogen fluoride);sodium nitrite at 0; for 10 h;Reagent/catalyst;Temperature;

Steps:

1-5 Example 1
1-aminocyclopropanecarboxylic acid (160.0g, 1.58mol, 1. Oequiv.) Was dissolved in triethylamine trihydrofluoride (700g, 4.74mol, 3.0equiv.), The temperature was controlled at 0 ° C, and Sodium nitrite (130.8g, 1.90mol, 1.2equiv.) Was added in batches. After the addition was completed and the reaction was completed at 0C for 10h, the system was slowly poured into 5L of ice water and extracted with ethyl acetate (400ml * 5). The phase was washed with saturated brine, dried over anhydrous Na2S04, filtered, and concentrated under reduced pressure to obtain crude 1-fluorocyclopropanecarboxylic acid. The crude product was added to petroleum ether for beating and suction filtration to obtain 1-fluorocyclopropanecarboxylic acid, a white solid, 62.6g, The yield is 38%.

References:

Nanjing He Ju Pharmaceutical Co., Ltd.;Pan Guojun;Chen Shulin CN110818552, 2020, A Location in patent:Paragraph 0035-0052

FullText