Tetrahydrofuran → HCID 12372976、化合物

HRID 48973

反応式

HRID 48973 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]([C:11]1[N:16]=[CH:15][CH:14]=[CH:13][N:12]=1)C#N.[H-].[Na+].[O:19]1CCCC1>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([C:11]1[N:16]=[CH:15][CH:14]=[CH:13][N:12]=1)=[O:19]

参加物

4

反応物 3

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 123729682-Chlorophenyl-(2-pyrimidinyl)acetonitrile

生成物 1

HCID 12372976HCID 12372976、化合物収率 64.7%

実験手順

A mixture of 2-chlorophenyl(2-pyrimidinyl)acetonitile (3.25 g, 0.0142 mol), sodium hydride (60% in mineral oil, 1.07 g, 0.016 mol) and anhydrous tetrahydrofuran is stirred two hours at reflux and cooled to room temperature. Dry air is bubbled into the mixture while stirring three days. The mixture is quenched by dropwise addition of a 3:1 water:methanol mixture and then water. The tetrahydrofuran is removed in vacuo and the aqueous residue filtered to afford the title compound as a brown solid (2.00 g, 64.7%) which is identified by NMR spectral analysis.

後処理

  1. temperatureat reflux
  2. customDry air
  3. customis bubbled into the mixture
  4. stirringwhile stirring three days
  5. customThe mixture is quenched by dropwise addition of a 3:1 water
  6. customThe tetrahydrofuran is removed in vacuo
  7. filtrationthe aqueous residue filtered

出典と根拠

ORDレコード
ord-10f9701d0dc8497f9978fdff41dd4fac
出典データセット
uspto-grants-2004_03
特許番号
US06706663B2

関連ノート

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