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Hydrochloric Acid → 1-(4-Phenyl-1,3-thiazol-2-yl)piperazine

HRID 2262988
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HRID 2262988 반응식
[C:1]1([C:7]2[N:8]=[C:9]([N:12]3[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14][CH2:13]3)[S:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.C(OCC)C>C(OCC)(=O)C>[C:1]1([C:7]2[N:8]=[C:9]([N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[S:10][CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 68777857Tert-butyl 4-(4-phenyl-1,3-thiazol-2-yl)piperazine-1-carboxylate

생성물 1

HCID 7124681-(4-Phenyl-1,3-thiazol-2-yl)piperazine수율 80.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

tert-Butyl 4-(4-phenyl-1,3-thiazol-2-yl)piperazine-1-carboxylate (691 mg, 2.00 mmol) was dissolved in ethyl acetate (50 ml), and a solution of 4 N hydrogen chloride in ethyl acetate (11 ml) was added thereto, followed by stirring at room temperature for 1 hour and half. Diethyl ether (20 ml) was poured to the reaction mixture, and a solid was separated by filtration, which was dissolved in an aqueous 1 N sodium hydroxide solution (7 ml). Water was poured to the reaction mixture, and the resulting solution was extracted with chloroform. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give 396 mg (80.8%) of the desired product as an oil.

후처리

  1. customa solid was separated by filtration, which
  2. dissolutionwas dissolved in an aqueous 1 N sodium hydroxide solution (7 ml)
  3. additionWater was poured to the reaction mixture
  4. extractionthe resulting solution was extracted with chloroform
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-7589fb7cb62749a891620c5bbd18c510
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07851473B2

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