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Thionyl Chloride → 2-(1-azidobut-3-enyl)-5-tosyl-5H-pyrrolo[2,3-b]pyrazine

HRID 1969528
ノート
印刷プレビュー

反応式

HRID 1969528 の反応式
[S:1]([N:11]1[C:15]2=[N:16][CH:17]=[C:18]([CH:20](O)[CH2:21][CH:22]=[CH2:23])[N:19]=[C:14]2[CH:13]=[CH:12]1)([C:4]1[CH:10]=[CH:9][C:7]([CH3:8])=[CH:6][CH:5]=1)(=[O:3])=[O:2].S(Cl)(Cl)=O.C([O-])(O)=O.[Na+].[N-:34]=[N+:35]=[N-:36].[Na+]>C(Cl)Cl.CCOC(C)=O>[N:34]([CH:20]([C:18]1[N:19]=[C:14]2[CH:13]=[CH:12][N:11]([S:1]([C:4]3[CH:10]=[CH:9][C:7]([CH3:8])=[CH:6][CH:5]=3)(=[O:3])=[O:2])[C:15]2=[N:16][CH:17]=1)[CH2:21][CH:22]=[CH2:23])=[N+:35]=[N-:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 24386Thionyl ChlorideHCID 33557Sodium AzideHCID 516892Sodium Bicarbonate2 回HCID 58557357HCID 58557357、化合物

生成物 1

HCID 585572372-(1-azidobut-3-enyl)-5-tosyl-5H-pyrrolo[2,3-b]pyrazine収率 101.3%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of 1-(5-tosyl-5H-pyrrolo[2,3-b]pyrazin-2-yl)but-3-en-1-ol (0.14 g, 0.41 mmol) in DCM (10 mL) was added thionyl chloride (0.045 mL, 0.61 mmol). The reaction mixture was stirred for about 8 h at ambient temperature and then EtOAc and saturated aqueous NaHCO3 (10 mL each) were added. The organic layer was separated, dried over anhydrous Na2SO4, filtered and concd in vacuo. The crude chloride was dissolved in DMF (10 mL) and sodium azide (0.159 g, 2.45 mmol) was added to the reaction mixture. The reaction mixture was stirred for about 15 h at ambient temperature and then EtOAc and saturated aqueous NaHCO3 (10 mL each) were added to the reaction mixture. The organic layer was separated, concd in vacuo, and purified by chromatography on silica gel eluting with 10-60% EtOAc in heptane to provide 2-(1-azidobut-3-enyl)-5-tosyl-5H-pyrrolo[2,3-b]pyrazine (0.153 g, 87%) as an oil: LC/MS (Table 1, Method a) Rt=2.84 min; MS m/z: 369 (M+H)+.

後処理

  1. customThe organic layer was separated
  2. dry with materialdried over anhydrous Na2SO4
  3. filtrationfiltered
  4. dissolutionThe crude chloride was dissolved in DMF (10 mL)
  5. stirringThe reaction mixture was stirred for about 15 h at ambient temperature
  6. customThe organic layer was separated
  7. customconcd in vacuo, and purified by chromatography on silica gel eluting with 10-60% EtOAc in heptane

出典と根拠

ORDレコード
ord-7f558fc3533640439f601258d14e8038
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426411B2

反応ノート

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