Chemiluminescent 1,2-dioxietanes
A dioxetane and single-ring technology, which is applied in the field of chemiluminescence 1,2-dioxetane with a power supply on the four-membered peroxide ring, can solve the problems of poor luminescence and the like
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[0081] This example illustrates that [(4-methoxy)-4-(3-phosphoryloxyphenyl)spiro[1,2-dioxetane-3,2′-adamantane-4,5-ene] Preparation method of disodium salt (46). The reaction sequence is as follows:
[0082] (a) Synthesis of 5-hydroxyadamantan-2-one (40)
[0083] In a single necked 500 mL round bottom flask equipped with a magnetic stirrer and water bath was added 75 parts of acetic acid containing 5 parts of acetic anhydride. 25 parts of chromium trioxide were added in portions over 40 minutes while maintaining the temperature at 15-20°C with a water bath. Add 5 parts of adamantan-2-one in portions over 15 minutes. Stirring was continued for 1 hour. The viscous reaction mixture was poured into cold 250 mL of 20% aqueous sodium hydroxide. The aqueous layer was extracted three times with 250 ml of ethyl acetate, and washed twice with 250 ml of water. Then dry over sodium sulfate. The solvent was distilled off under reduced pressure and chromatographed on a silica gel col...
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