반응 #6000

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pivaloyl chloride

N-carbobenzoxydopamine

sodium carbonate

→

desired compound

수율 80.1%

3,4-di-O-pivaloyl-N-carbobenzoxydopamine

수율 80.1%

용매

pyridine

반응 조건

후처리

1. 1
   기타to react at 35° to 40° C. for 3 hours
2. 2
   workup.ADDITIONFurther, the reaction mixture was poured into ice
3. 3
   추출After extracting with diethyl ether
4. 4
   건조drying over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off
6. 6
   기타to give crude crystals
7. 7
   기타The resulting crude crystals then recrystallized from petroleum ether

실험 절차

To 150 ml of a pyridine solution containing 23.0 g (98 mmol) of N-carbobenzoxydopamine obtained in Synthetic Example 1-(1), was added 24.1 g (200 mmol) of pivaloyl chloride dropwise at 5° to 10° C. After stirring at room temperature for 12 hours, the mixture was allowed to react at 35° to 40° C. for 3 hours. Further, the reaction mixture was poured into ice and a sodium carbonate solution and the stirring was continued at room temperature for 30 minutes. After extracting with diethyl ether and drying over anhydrous magnesium sulfate, the solvent was distilled off to give crude crystals. The resulting crude crystals then recrystallized from petroleum ether to obtain 27.1 g (yield: 80.1%) of the desired compound in the form of white crystals

출처