(Carbethoxymethylene)triphenylphosphorane-13C2 synthesis

Yield:90830-64-1 87%

Reaction Conditions:

in toluene at 20 - 30; for 16 h;

Steps:

5 5: Synthesis of compound 5

Dissolve triphenylphosphine (38mmol, 10g) in toluene (50mL), add ethyl bromoacetate-13C2 (23.7mmol, 4g) dropwise at a rate of 1 to 2 drops/sec. After the addition is complete, at 20~ Stir and react for 16 hours at 30°C. Remove toluene by rotary evaporation under reduced pressure. Add 50mL of dichloromethane to dissolve it, then add 10wt% sodium hydroxide solution to adjust pH≈10, stir and separate into layers. After drying with sodium sulfate, the methylene chloride was removed by rotary evaporation under reduced pressure to obtain compound 5,

References:

CN113004300,2021,A Location in patent:Paragraph 0047; 0060-0061