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Sodium Methoxide → HCID 9922442, 화합물

HRID 1795861
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HRID 1795861 반응식
[C:1]1([C:7]2[C:15]([C:16]3[CH:17]=[N:18][C:19](S(C4C=CC=CC=4)(=O)=O)=[CH:20][CH:21]=3)=[C:10]3[CH:11]=[N:12][CH:13]=[CH:14][N:9]3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:31][O-:32].[Na+]>CO.O1CCOCC1>[CH3:31][O:32][C:19]1[N:18]=[CH:17][C:16]([C:15]2[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[N:8][N:9]3[CH:14]=[CH:13][N:12]=[CH:11][C:10]=23)=[CH:21][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10942334Sodium MethoxideHCID 22180671HCID 22180671, 화합물

생성물 1

HCID 9922442HCID 9922442, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

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온도
85 °C

실험 절차

A mixture of 2-phenyl-3-[6-(phenylsulfonyl)-3-pyridinyl]pyrazolo[1,5-a]pyrazine (3.93 g) and sodium methoxide (5.2M MeOH solution, 10 mL) in MeOH (60 mL) and 1,4-dioxane (60 mL) was stirred at 85° C. for 1 h. The reaction mixture was concentrated in vacuo, and ice water was added, extracted, with EtOAc, washed with water and brine, dried over sodium sulfate, evaporated in vacuo. The residue was purified by silica gel column chromatography (n-hexane-EtOAc 2:3) to give 3-(6-methoxy-3-pyridinyl)-2-phenylpyrazolo[1,5-a]pyrazine (2.37 g) as an oil.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo, and ice water
  2. additionwas added
  3. extractionextracted, with EtOAc
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by silica gel column chromatography (n-hexane-EtOAc 2:3)

출처 및 근거

ORD 기록
ord-759b6e827389444880d8138bcfaff4bd
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030121B2

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