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Piperazine → HCID 10982183, 화합물

HRID 1603587
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HRID 1603587 반응식
Br[C:2]1[CH:7]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:5]=[C:4]([Br:18])[N:3]=1.[NH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C(N(CC)CC)C>O1CCOCC1>[Br:18][C:4]1[CH:5]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:7]=[C:2]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4837PiperazineHCID 8471TriethylamineHCID 110146744-[(2,6-Dibromo-4-pyridinyl)sulfonyl]aniline

생성물 1

HCID 10982183HCID 10982183, 화합물수율 82.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
40 °C

실험 절차

0.275 g (0.0007 mol) of 4-(2,6-dibromopyridine-4-sulphonyl)-phenylamine was dissolved in 10 ml of dioxane and treated with 0.066 g (0.00077 mol) of piperazine and 1 ml of triethylamine. The mixture was stirred at 40° C. for 72 hrs. and the solvent was then removed. The residue was partitioned in ethyl acetate and water and the organic phase was extracted with sat. sodium chloride solution and dried over MgSO4 and filtered. After removal of the solvent the residue was chromatographed on silica gel with dichloromethane/methanol 9:1 and there was obtained 0.23 g (82%) of 4-(2-bromo-6-piperazin-1-ylpyridin-4-sulphonyl) -phenylamine as yellowish crystals; m.p.: 173-175° C.

후처리

  1. customand the solvent was then removed
  2. customThe residue was partitioned in ethyl acetate
  3. extractionwater and the organic phase was extracted with sat. sodium chloride solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customAfter removal of the solvent the residue
  7. customwas chromatographed on silica gel with dichloromethane/methanol 9:1

출처 및 근거

ORD 기록
ord-1f8bb73f991f4c5bb070ff7f5bddebe2
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05990105

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