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Water → HCID 68776951, 화합물

HRID 2262973
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HRID 2262973 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([N:10]([C:19]([O:21]CC(Cl)(Cl)Cl)=O)C(OCC(Cl)(Cl)Cl)=O)=[N:2]1.[C:27]1([C:33]2[N:37]=[C:36]([N:38]3[CH2:43][CH2:42][NH:41][CH2:40][CH2:39]3)[S:35][N:34]=2)[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.C(N(C(C)C)CC)(C)C.O>CS(C)=O>[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([NH:10][C:19]([N:41]2[CH2:42][CH2:43][N:38]([C:36]3[S:35][N:34]=[C:33]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[N:37]=3)[CH2:39][CH2:40]2)=[O:21])=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 27777601-(3-Phenyl-(1,2,4)thiadiazol-5-yl)-piperazineHCID 86625482HCID 86625482, 화합물

생성물 1

HCID 68776951HCID 68776951, 화합물수율 12.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide
용매

실험 절차

A mixed solution of bis(2,2,2-trichloroethyl) 1H-indazol-3-ylimidodicarbonate (295 mg, 0.61 mmol), 1-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine (300 mg, 1.22 mmol) and diisopropylethylamine (0.106 ml, 0.610 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 80° C. for 5 hours. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (100% ethyl acetate, followed by ethyl acetate:methanol=1:1) and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 30.2 mg (12.2%) of the desired product as a solid.

후처리

  1. extractionthe resulting solution was extracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (100% ethyl acetate, followed by ethyl acetate:methanol=1:1)
  6. customrecrystallized from a mixed solvent of hexane and tetrahydrofuran

출처 및 근거

ORD 기록
ord-50f4208900f44522bc1f07738ae4758a
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07851473B2

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