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Example 4
Application process: 35% perchloric acid aqueous solution was added dropwise to a solution of compound A (80g) in ether (1000mL) at room temperature , and then stirred overnight
The R&D personnel immediately discussed with the supervisor, and the modified operation description was as follows: At room temperature, 35% perchloric acid aqueous solution was added dropwise to a solution of compound A (80g) in ether (1000mL), and then stirred overnight
Finally, the response was approved
Example 5
Application process: At 25℃, add azobisisobutyronitrile (AIBN) and N-bromosuccinimide (NBS) to compound A, diethyl phosphate and N, N-diisopropyl at one time Diethylamine (DIPEA) in the mixed liquid, and then the temperature is raised to 65-75°C
Remarks: This is a free radical reaction.
Example 6
Application process: Dissolve the reaction substrate A and RuCl 3 ·H 2 O in a mixture of acetonitrile, EtOAc and H 2 O according to the prescribed amount, add NaIO4 in batches under an ice water bath, and control the internal temperature of the reaction at 10~25℃ After adding, stir overnight at room temperature
Remarks: Use sodium sulfite or sodium thiosulfate to quench excess sodium periodate