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With water; potassium hydroxide In ethanol for 24h; Reflux;
2-7 Example 2-1
General procedure: Compound 1-(3-fluorophenyl)cyclopropane-1-carbonitrile (6.85 g, 42.5 mmol)Dissolved in 34ml of ethanol,An aqueous solution (34 ml) of potassium hydroxide (7.154 g, 127.5 mmol) was added,Heated to reflux for 24 hours,After the reaction, the solvent was concentrated to dryness,The residue was dissolved in 15ml of water, and the pH value was adjusted to 3-4 with hydrochloric acid solution,A white solid precipitated out, filtered and washed the filter cake with water,Dry to obtain compound 1-(3-fluorophenyl)cyclopropane-1-carboxylic acid (7.18g), yield 93.7%,
2
[ 186347-65-9 ]
[ 186347-67-1 ]
Yield
Reaction Conditions
Operation in experiment
Stage #1: 1-(3,4-difluoro-phenyl)-cyclopropanecarbonitrile With sodium hydroxide; water for 2.5h; Heating / reflux;
Stage #2: With hydrogenchloride In water at 0℃;
18
1- (3, 4-Difluoro-phenyl)-cyclopropanecarboxylic acid.; The 1- (3, 4-Difluoro-phenyl) - cyclopropanecarbonitrile (4.9 g crude from last step) was refluxed in sodium hydroxide (10 % aqueous solution, 100 mL) for 2. 5 hours. The reaction mixture was washed twice with ethyl ether (100 mL). The aqueous phase was cooled to 0 °C and brought to between pH 2 and 3 with concentrated hydrochloric acid. The aqueous layer was then extracted twice with ethyl acetate (100 mL). The combined organic layers were dried with anhydrous sodium sulfate, filtered, and evaporated to dryness to give a white solid (4.0 g, 20 mmol, 43.5 %, two steps). ESI-MS ln/z calc. 198.05, found 197.05 (M-Ht 1H w (CDC13) : 8 10.9 (br. s, 1 H), 7.16-7. 02 (m, 3 H), 1.66-1. 60 (m, 2 H), 1.27-1. 21 (m, 2 H)
With lithium hydroxide In water; ethylene glycol at 100℃; for 24h;
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