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Iodoethane → HCID 44200192、化合物

HRID 600389
ノート
印刷プレビュー

反応式

HRID 600389 の反応式
[CH3:1][C:2]([CH3:24])([CH3:23])[C:3]([C:5]1[C:13]2[NH:12][C:11](=[O:14])[CH:10]=[N:9][C:8]=2[N:7](COCC[Si](C)(C)C)[CH:6]=1)=[O:4].I[CH2:26][CH3:27].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:26]([O:14][C:11]1[N:12]=[C:13]2[C:5]([C:3](=[O:4])[C:2]([CH3:1])([CH3:23])[CH3:24])=[CH:6][NH:7][C:8]2=[N:9][CH:10]=1)[CH3:27]
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 6340IodoethaneHCID 11430Potassium CarbonateHCID 57831039HCID 57831039、化合物

生成物 1

HCID 44200192HCID 44200192、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 7-(2,2-dimethyl-propionyl)-5-(2-trimethylsilanyl-ethoxymethyl)-1,5-dihydro-pyrrolo[2,3-b]pyrazin-2-one (0.080 g, 0.23 mmol), iodoethane (0.018 mL, 0.24 mmol) and potassium carbonate (0.038 g, 0.28 mmol) in 3 mL of acetone was stirred at reflux overnight, then concentrated. The residue was partitioned between 30 mL of ethyl acetate and 30 mL of water. The organic layer was dried over MgSO4, filtered and concentrated to 0.075 g (86%) of crude 1-[2-ethoxy-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-2,2-dimethyl-propan-1-one as a yellow oil that was used without further purification.

後処理

  1. temperatureat reflux overnight
  2. concentrationconcentrated
  3. customThe residue was partitioned between 30 mL of ethyl acetate and 30 mL of water
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated to 0.075 g (86%) of crude 1-[2-ethoxy-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-2,2-dimethyl-propan-1-one as a yellow oil that
  7. customwas used without further purification

出典と根拠

ORDレコード
ord-7b00bd963476481c8c2f5426e5f0590c
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07902197B2

反応ノート

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