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Tetrahydrofuran → 2,4-Bis(acrylamido)-6-ethoxypyrimidine

HRID 2353811
ノート
印刷プレビュー

反応式

HRID 2353811 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([O:9][CH2:10][CH3:11])[N:3]=1.[C:12](Cl)(=[O:15])[CH:13]=[CH2:14].C(N(CC)CC)C.[O:24]1C[CH2:27][CH2:26][CH2:25]1>>[C:12]([NH:1][C:2]1[N:7]=[C:6]([NH:8][C:25](=[O:24])[CH:26]=[CH2:27])[CH:5]=[C:4]([O:9][CH2:10][CH3:11])[N:3]=1)(=[O:15])[CH:13]=[CH2:14]
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 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 2226632,4-Diamino-6-ethoxypyrimidine

生成物 1

HCID 113115502,4-Bis(acrylamido)-6-ethoxypyrimidine

実験手順

1.54 g (10 mmols) of the product obtained by the procedure described in (1b) are reacted with 1.8 mL of acryloyl chloride, in the presence of 4.2 mL of triethylamine in 100 mL of tetrahydrofuran. The addition is performed dropwise and under cooling in an ice bath. After the addition is complete, the reaction mixture is stirred at room temperature for several hours. The solvent is evaporated under vacuum and then 100 mL of water are added to the solid residue to dissolve the TEA.HCl salt. The mixture is then extracted with 3×100 mL CHCl3, the organic phases are combined, dried over MgSO4 and the solvent is finally evaporated in vacuo. A white solid is finally obtained and there is no need for further purification.

後処理

  1. additionThe addition
  2. temperatureunder cooling in an ice bath
  3. additionAfter the addition
  4. customThe solvent is evaporated under vacuum
  5. addition100 mL of water are added to the solid residue
  6. dissolutionto dissolve the TEA
  7. extractionThe mixture is then extracted with 3×100 mL CHCl3
  8. dry with materialdried over MgSO4
  9. customthe solvent is finally evaporated in vacuo
  10. customA white solid is finally obtained
  11. customfor further purification

出典と根拠

ORDレコード
ord-25172287367a49a38ccbccc3d128718c
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07750090B2

反応ノート

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