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ChemicalBook CAS DataBase List 2,4,6-TRICHLORO-5-FLUOROPYRIMIDINE
6693-08-9

2,4,6-TRICHLORO-5-FLUOROPYRIMIDINE synthesis

5synthesis methods
-

Yield:6693-08-9 55%

Reaction Conditions:

with trichlorophosphate in N,N-dimethyl-aniline at 110; for 8 h;Inert atmosphere;

Steps:

1.2 Step 2: Synthesis of Intermediate Int-2
The intermediates Int-1 (95g, 650mmol), POCl3 (425ml, 6552mmol) and 83ml of N,N-dimethylaniline were slowly added dropwise to the round bottom flask under nitrogen conditions, and then stirred under reflux at 110° C. for 8 hours. After the reaction is over, cool it to room temperature and slowly pour the reactant into excess ice water (beware of severe exothermic reaction). After extraction with ethyl acetate and drying with MgSO4, filter. The filtrate was distilled under reduced pressure to obtain 72 g (55%) of an intermediate Int-2.

References:

Samsung SDI Co., Ltd;Kim Chang-u;Kim Hyeong-seon;Ryu Dong-wan;Shin Chang-ju;Lee Seung-jae;Lee Mi-jin;Lee Hyeon-gyu;Jeong Seong-hyeon;Jeong Ho-guk KR2020/86131, 2020, A Location in patent:Paragraph 0311-0312; 0316-0317

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