Hydrochloric Acid → 1-(3-Pyridin-2-yl-1,2,4-thiadiazol-5-yl)piperazine

HRID 2262982노트

반응식

HRID 2262982 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:11]=[C:10]([N:12]2[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]2)[S:9][N:8]=1.Cl.CCCCCC>O1CCCC1.C(OCC)(=O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:11]=[C:10]([N:12]2[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]2)[S:9][N:8]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 8058HexaneHCID 68782158HCID 68782158, 화합물

생성물 1

HCID 687780931-(3-Pyridin-2-yl-1,2,4-thiadiazol-5-yl)piperazine

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

tert-Butyl 4-(3-pyridin-2-yl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxylate (6.35 g, 17.0 mmol) was dissolved in tetrahydrofuran (100 ml), and a solution of 4 N hydrogen chloride in ethyl acetate (50 ml) was added thereto, followed by stirring at room temperature for 5 hours. Hexane (250 ml) was poured to the reaction mixture, and a solid was separated by filtration. The obtained solid was dissolved in an aqueous saturated sodium hydrogen carbonate solution, followed by stirring at room temperature for 2 hours. Water was poured to the reaction mixture, and the resulting solution was extracted with a mixed solution of ethyl acetate/tetrahydrofuran (1:1). The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Hexane was added to the residue, and 2.79 g (67.0%) of the desired product as a solid was separated by filtration.

후처리

  1. customa solid was separated by filtration
  2. dissolutionThe obtained solid was dissolved in an aqueous saturated sodium hydrogen carbonate solution
  3. stirringby stirring at room temperature for 2 hours
  4. additionWater was poured to the reaction mixture
  5. extractionthe resulting solution was extracted with a mixed solution of ethyl acetate/tetrahydrofuran (1:1)
  6. washThe extract was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure
  9. additionHexane was added to the residue, and 2.79 g (67.0%) of the desired product as a solid
  10. customwas separated by filtration

출처 및 근거

ORD 기록
ord-9d04af373dac46e4a36136af01991004
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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