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ChemicalBook CAS DataBase List 4-CHLORO-5H-PYRROLO[3,2-D] PYRIMIDINE

4-CHLORO-5H-PYRROLO[3,2-D] PYRIMIDINE synthesis

6synthesis methods
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Yield:84905-80-6 93.2%

Reaction Conditions:

with 1,4-diaza-bicyclo[2.2.2]octane;triethylamine;trichlorophosphate in toluene at 50; for 15 h;Temperature;Reagent/catalyst;Solvent;

Steps:

1.3-8.3 (3) Formula I - Synthesis of 4-chloropyrrolopyrimidine:

Adding 4-hydroxypyrrolopyrimidine to 1000 ml of toluene to form an organic mixed solution of 4-hydroxypyrrolopyrimidine;After adding a chlorinating reagent-triethylenediamine to the organic mixed solution of 4-hydroxypyrrolopyrimidine, the temperature is raised to 50 ° C.Adding organic lye triethylamine,After the completion of the dropwise addition, the temperature was raised to 50 ° C, and the reaction was further concentrated for 15 hours. The concentrate was poured into ice water, the pH was adjusted to 7-8 with sodium carbonate, and the solid was collected by filtration. The solid was dissolved in acetone, decolorized, and recrystallized. White solid 4-chloropyrrolopyrimidine in a yield of 93.2%. The total yield was 77.3% and the purity was greater than 99.1%.

References:

CN109824675,2019,A Location in patent:Page/Page column 7-12

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