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Hydrochloric Acid → HCID 178526697, 화합물

HRID 1710928
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HRID 1710928 반응식
[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[N:15]=[CH:16][N:17](COCC[Si](C)(C)C)[CH:18]=3)[S:13][C:6]=12.Cl>CCO>[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-:33])=[O:32])[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]2[CH:11]=[C:12]([C:14]3[N:15]=[CH:16][NH:17][CH:18]=3)[S:13][C:6]=12
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

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HCID 313Hydrochloric AcidHCID 594245697-(2-Fluoro-4-nitrophenoxy)-2-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazol-4-yl)thieno[3,2-b]pyridine

생성물 1

HCID 178526697HCID 178526697, 화합물수율 100%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
85 °C

실험 절차

To a suspension of 92 (3.3 g, 6.8 mmol) in EtOH (8 ml) was added concentrated HCl (7 ml) and distilled water (4 ml). The mixture was heated at 80-90° C. for 2.5 h, cooled to room temperature and concentrated under reduced pressure. The remaining residue was subjected to azeotropic distillation with EtOH followed by neutralization with saturated aqueous NaHCO3. The solid that precipitated was filtered and washed with water, and the filtrate was extracted with EtOAc. The solid and EtOAc extract were combined, evaporated under reduced pressure and the residue was collected and dried to afford the title compound 93 (2.4 g, 100% yield) as a yellow solid. MS (m/z) 357.0 (M+H).

후처리

  1. distillationdistilled water (4 ml)
  2. temperaturecooled to room temperature
  3. concentrationconcentrated under reduced pressure
  4. distillationThe remaining residue was subjected to azeotropic distillation with EtOH
  5. customThe solid that precipitated
  6. filtrationwas filtered
  7. washwashed with water
  8. extractionthe filtrate was extracted with EtOAc
  9. extractionThe solid and EtOAc extract
  10. customevaporated under reduced pressure
  11. customthe residue was collected
  12. customdried

출처 및 근거

ORD 기록
ord-704fa0b9e9e14e88a326913748c78a6f
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790729B2

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