Phosphorus oxychloride → 2-chloro-6-(trifluoromethyl)-1H-benzimidazole
反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:12]=[CH:11][C:6]2[NH:7][C:8](=O)[NH:9][C:5]=2[CH:4]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:8]1[NH:9][C:5]2[CH:4]=[C:3]([C:2]([F:14])([F:13])[F:1])[CH:12]=[CH:11][C:6]=2[N:7]=1参加物
3
実験手順
A solution of the dihydrobenzoimidazol-2-one from step (b) above (2.02 g, 10 mmol) in POCl3 (30 mL) was heated at 95° C. for 16 h. The reaction mixture was cooled to room temperature, the solvent was removed in vacuo and the resulting oily residue subjected to azeotropic distillation with toluene (3×50 mL) at 50° C. The crude product was dissolved in EtOAc (50 mL), washed with brine (10 mL) then dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was recrystallized from EtOAc/hexane to give the title compound.
後処理
- customthe solvent was removed in vacuo
- distillationthe resulting oily residue subjected to azeotropic distillation with toluene (3×50 mL) at 50° C
- dissolutionThe crude product was dissolved in EtOAc (50 mL)
- washwashed with brine (10 mL)
- dry with materialthen dried over Na2SO4
- filtrationfiltered
- customThe solvent was removed in vacuo
- customthe residue was recrystallized from EtOAc/hexane
出典と根拠
- ORDレコード
- ord-5c21a7033d1d4fd2aedf69f95dde0f89
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08026241B2
反応ノート
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