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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 70255947, 화합물 → 7-Fluoro-2,3-dihydro-1H-cyclopenta[b]quinolin-9-amine

HRID 366393
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HRID 366393 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH2:13][CH2:12][CH2:11][C:10]=2[C:14]#[N:15])=[CH:4][CH:3]=1>[Ti](Cl)(Cl)(Cl)Cl.[OH-].[Na+]>[NH2:15][C:14]1[C:4]2[CH:3]=[C:2]([F:1])[CH:7]=[CH:6][C:5]=2[N:8]=[C:9]2[CH2:13][CH2:12][CH2:11][C:10]=12
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참가 물질

4

반응물 1

HCID 70255947HCID 70255947, 화합물

생성물 1

HCID 232898317-Fluoro-2,3-dihydro-1H-cyclopenta[b]quinolin-9-amine

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 14798Sodium Hydroxide용매

반응 조건

온도
140 °C

실험 절차

Under nitrogen, titanium tetrachloride (1.2 ml, 11 mmol) was added to the above enamine (Example 20) (2.0 g, 10 mmol) and the stirred mixture was heated at 140° C. for 1 hour. After cooling, 10M-sodium hydroxide solution (20 ml) was added and the mixture heated under reflux for 1 hour. After being allowed to cool, this mixture was filtered and the solids washed with dichloromethane. Any organics in the filtrate were also extracted into dichloromethane. All extracts were combined, dried (Na2SO4), filtered and the solvent evaporated. Kugelrohr distillation (175° C., 0.05 mmHg) gave the product as an off-white powder.

후처리

  1. temperatureAfter cooling
  2. temperaturethe mixture heated
  3. temperatureunder reflux for 1 hour
  4. temperatureto cool
  5. filtrationthis mixture was filtered
  6. washthe solids washed with dichloromethane
  7. extractionAny organics in the filtrate were also extracted into dichloromethane
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. customthe solvent evaporated
  11. distillationKugelrohr distillation (175° C., 0.05 mmHg)

출처 및 근거

ORD 기록
ord-7560a5182b6b48c4a429d23fadffba43
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06130228

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