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[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]=1참가 물질
3
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-2eaab8ce31e44ef193d5a21e9388dd8c
- 출처 데이터셋
- uspto-grants-2009_09
- 특허 번호
- US07582761B2
연결된 노트
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