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Sodium hydride → 5-Bromo-2-(2-pyrrolidin-1-yl-ethoxy)-pyrimidine

HRID 888041
ノート
印刷プレビュー

反応式

HRID 888041 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[CH2:8][CH2:7][CH2:6][CH2:5]1.[Br:9][C:10]1[CH:11]=[N:12][C:13](Cl)=[N:14][CH:15]=1.[H-].[Na+]>CN(C=O)C>[Br:9][C:10]1[CH:11]=[N:12][C:13]([O:1][CH2:2][CH2:3][N:4]2[CH2:8][CH2:7][CH2:6][CH2:5]2)=[N:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 762881-PyrrolidineethanolHCID 6066655-Bromo-2-chloropyrimidine

生成物 1

HCID 638675465-Bromo-2-(2-pyrrolidin-1-yl-ethoxy)-pyrimidine収率 38%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of N-2-hydroxyethylpyrrolidine (0.9 ml, 7.71 mmol) and 5-bromo-2-chloropyrimidine (1.2 g, 6.20 mmol), in DMF (7 ml), was added sodium hydride (60% in mineral oil, 0.35 g, 8.75 mmol). The mixture was stirred, under argon, at ambient temperature for 1 hour, before being heated to 90° C. and stirred for a further hour. The reaction mixture was then partitioned between ethyl acetate and water. The organics were separated, dried over magnesium sulfate and evaporated to dryness. The resultant oil was purified by flash chromatography on silica, eluting with an increasing gradient of methanol in dichloromethane (which contained 1% aqueous ammonia solution, 0.88 M) to give the title compound (640 mg, 38%); NMR Spectrum: (CDCl3) 1.76 (m, 4H), 2.39 (m, 4H), 3.90 (t, 2H), 4.48 (t, 2H), 8.50 (s, 2H); Mass Spectrum: M+H+ 272.

後処理

  1. temperaturebefore being heated to 90° C.
  2. stirringstirred for a further hour
  3. customThe reaction mixture was then partitioned between ethyl acetate and water
  4. customThe organics were separated
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness
  7. customThe resultant oil was purified by flash chromatography on silica
  8. washeluting with an increasing gradient of methanol in dichloromethane (which contained 1% aqueous ammonia solution, 0.88 M)

出典と根拠

ORDレコード
ord-0844d7b57d664ae097e9cee74c7b12d9
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08247562B2

反応ノート

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