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Hydrochloric Acid → 2-Chloro-6-(4-piperidinyloxy)pyrazine

HRID 1357609
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HRID 1357609 반응식
Cl.[Cl:2][C:3]1[N:8]=[C:7]([O:9][CH:10]2[CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11]2)[CH:6]=[N:5][CH:4]=1>CO>[Cl:2][C:3]1[CH:4]=[N:5][CH:6]=[C:7]([O:9][CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[N:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21906088tert-Butyl 4-((6-chloropyrazin-2-yl)oxy)piperidine-1-carboxylate

생성물 1

HCID 181869152-Chloro-6-(4-piperidinyloxy)pyrazine

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

Aqueous 3.0 M HCl (12 mL) was added to a solution of the product obtained in Step 1 above (5.00 g, 15.9 mmol) in methanol (200 mL). The reaction mixture was stirred at 50° C. for 5 h and concentrated in vacuo. The residue was dissolved in water (50 mL) and basified with K3PO4. The aqueous phase was extracted with ethyl acetate (5×40 mL), dried (MgSO4), and concentrated in vacuo. This gave 3.08 g (91%) of the title compound as a colorless oil which slowly decomposed upon standing. HRMS m/z calcd for C9H12ClN3O (M)+ 213.0669, found 213.0663.

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후처리

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in water (50 mL)
  3. extractionThe aqueous phase was extracted with ethyl acetate (5×40 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3bdd815baaf8424e84d313f9a0fd94db
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06593330B2

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