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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 67367246, 화합물 → HCID 67367265, 화합물

HRID 1676231
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HRID 1676231 반응식
C([O:8][C:9]1[CH:14]=[CH:13][N:12]([C:15]2[CH:22]=[CH:21][C:18]([C:19]#[N:20])=[CH:17][C:16]=2[F:23])[C:11](=[O:24])[CH:10]=1)C1C=CC=CC=1>[Pd].CO>[F:23][C:16]1[CH:17]=[C:18]([CH:21]=[CH:22][C:15]=1[N:12]1[CH:13]=[CH:14][C:9]([OH:8])=[CH:10][C:11]1=[O:24])[C:19]#[N:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 67367246HCID 67367246, 화합물

생성물 1

HCID 67367265HCID 67367265, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To 4-(4-(benzyloxy)-2-oxopyridin-1(2H)-yl)-3-fluorobenzonitrile (250 mg, 0.780 mmol) and 10% palladium on carbon (50 mg, 0.470 mmol) was applied vacuum then placed under an atmosphere of nitrogen. Methanol (5 mL) was added and vacuum applied briefly. The reaction was placed under an atmosphere of hydrogen for 6 hours. The reaction mixture was passed through a 10×10 mm CELITE® 545 filter aid plug eluting with an additional 10 mL each of MeOH and CH2Cl2. The filtrate was concentrated to 170 mg of a pale tan foam. Added 5 mL MeOH and heated to reflux, filtered hot and rinsed with 3×2 mL warm MeOH. The filtrate was concentrated to crude product (166 mg, 0.577 mmol, 74%) as a pale yellow solid which was used as obtained in the subsequent step. MS (ESI) 231.1 (M+1).

후처리

  1. filtrationfilter aid plug
  2. washeluting with an additional 10 mL each of MeOH and CH2Cl2
  3. concentrationThe filtrate was concentrated to 170 mg of a pale tan foam
  4. additionAdded 5 mL MeOH
  5. temperatureheated
  6. temperatureto reflux
  7. filtrationfiltered hot
  8. washrinsed with 3×2 mL
  9. temperaturewarm MeOH
  10. customas obtained in the subsequent step

출처 및 근거

ORD 기록
ord-b2010b88ee804906b468732f5c8a88ec
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08003796B2

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