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Toluene → HCID 20290694, 화합물

HRID 1413759
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HRID 1413759 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[C:13](=[O:14])[N:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]2=[N:6]1.C1(C)C=CC=CC=1.[Cl:22][C:23]1[N:28]=[C:27]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)[CH:26]=[N:25][CH:24]=1>C(N(CC)CC)C>[ClH:1].[Cl:22][C:23]1[N:28]=[C:27]([N:29]2[CH2:30][CH2:31][N:32]([CH2:2][CH2:3][CH2:4][N:5]3[C:13](=[O:14])[N:8]4[CH:9]=[CH:10][CH:11]=[CH:12][C:7]4=[N:6]3)[CH2:33][CH2:34]2)[CH:26]=[N:25][CH:24]=1
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참가 물질

5

반응물 3

HCID 1140TolueneHCID 1079922-Chloro-6-(1-piperazinyl)pyrazineHCID 130412482-(3-Chloropropyl)[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one

생성물 1

HCID 20290694HCID 20290694, 화합물

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To a solution of 3.2 g. (15.1 mmole) of 2-(3-chloropropyl)-1,2,4-triazolo[4,3-a]pyridin-3(2H)-one in 25 ml. toluene is added 2.4 g. (12.1 mmole) of 6-chloro-2-(1-piperazinyl)pyrazine and 2.1 ml. triethylamine. The mixture is refluxed 3 days under N2, cooled, and filtered to give 1.85 g. of the crude base of the title compound. The crude base is chromatographed on silica gel to give the pure base on elution with 1-2% methanol-chloroform. This material is dissolved in absolute ethanol and the solution treated with anhydrous hydrogen chloride to give tan crystals of title compound, m.p. 243°-245°, dec.

후처리

  1. temperatureThe mixture is refluxed 3 days under N2
  2. temperaturecooled
  3. filtrationfiltered
  4. customto give 1.85 g

출처 및 근거

ORD 기록
ord-b1b2325b47434ace888c9daeb4c51bc7
출처 데이터셋
uspto-grants-1981_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04251530

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