Piperidine → 5-Bromo-2-(piperidin-1-yl)pyrimidine

HRID 641453노트

반응식

HRID 641453 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Br:7][C:8]1[CH:9]=[N:10][C:11](Cl)=[N:12][CH:13]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1.C(OCC)(=O)C>[Br:7][C:8]1[CH:9]=[N:10][C:11]([N:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)=[N:12][CH:13]=1

참가 물질

6

반응물 3

HCID 8082PiperidineHCID 8471TriethylamineHCID 6066655-Bromo-2-chloropyrimidine

생성물 1

HCID 36146825-Bromo-2-(piperidin-1-yl)pyrimidine

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

Piperidine (5.1 ml, 51.6 mmol) was added to a stirred solution of 5-bromo-2-chloropyrimidine (5 g, 25.8 mmol) and triethylamine (9.0 ml, 64.5 mmol) in toluene (30 ml). After stirring at room temperature for 24 hours the reaction mixture was diluted with ethyl acetate and washed with 2N hydrochloric acid, brine and dried (magnesium sulfate). The organic layer was filtered, concentrated in vacuo and the resulting residue was purified by column chromatography eluting with ethyl acetate to afford the title compound (D32).

후처리

  1. washwashed with 2N hydrochloric acid, brine
  2. dry with materialdried (magnesium sulfate)
  3. filtrationThe organic layer was filtered
  4. concentrationconcentrated in vacuo
  5. customthe resulting residue was purified by column chromatography
  6. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-d900d825718f443d8c7afdae809cbd9e
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696193B2

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