Tetrahydrofuran → HCID 12372976, 화합물

HRID 48973

반응식

HRID 48973 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 12372976HCID 12372976, 화합물수율 64.7%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10f9701d0dc8497f9978fdff41dd4fac
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706663B2

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