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

HRID 645785ノート

反応式

HRID 645785 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2929ed84d2064fb4b7fa679eb0965b5b
出典データセット
uspto-grants-2010_04
特許番号
US07704994B2

反応ノート

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