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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Piperidine → HCID 66655979, 화합물

HRID 1505472
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HRID 1505472 반응식
N[C:2]1[C:3]2[C:27]3([CH2:31][CH2:30]OC3)[C:26](=[O:32])[NH:25][C:4]=2[N:5]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[N:10]([CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[N:9]=2)[N:7]=1.N1CCCC[CH2:34]1>CC(C)=O.C(OCC)(=O)C>[F:24][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[CH2:17][N:10]1[C:11]2=[N:12][CH:13]=[CH:14][CH:15]=[C:16]2[C:8]([C:6]2[N:7]=[CH:2][C:3]3[C:27](=[C:31]([CH3:34])[CH3:30])[C:26](=[O:32])[NH:25][C:4]=3[N:5]=2)=[N:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8082PiperidineHCID 56598426HCID 56598426, 화합물

생성물 1

HCID 66655979HCID 66655979, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

실험 절차

500 mg (1.388 mmol) of Example 4 were initially charged in acetone (50 ml), 0.274 ml (2.775 mmol) of piperidine was added and the mixture was heated under reflux for 1 h. After cooling, a precipitate was filtered off and washed with acetone, and the filtrate was concentrated under reduced pressure. This residue was then purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate gradient). The material obtained in this manner was once more slurried in ethyl acetate, filtered off, washed with ethyl acetate and dried under high vacuum. This gave 101 mg of the title compound as a solid (18% of theory).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 h
  3. temperatureAfter cooling
  4. filtrationa precipitate was filtered off
  5. washwashed with acetone
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThis residue was then purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate gradient)
  8. customThe material obtained in this manner
  9. filtrationfiltered off
  10. washwashed with ethyl acetate
  11. customdried under high vacuum

출처 및 근거

ORD 기록
ord-8eebc0489ef9409e9a320a1e9fceff98
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216978B2

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