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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Chf-1024 → HCID 19352272, 화합물

HRID 726889
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HRID 726889 반응식
[CH3:1][O:2][C:3]([NH:5][CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([O:18][CH3:19])[C:12]=2[O:16][CH3:17])[C:7]1=O)=[O:4].Cl.OC1C(O)=CC=C2C=1CCC(NC)C2>CO.[Pd]>[CH3:1][O:2][C:3]([NH:5][CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([O:18][CH3:19])[C:12]=2[O:16][CH3:17])[CH2:7]1)=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6918482Chf-1024HCID 19352269HCID 19352269, 화합물

생성물 1

HCID 19352272HCID 19352272, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

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온도
30 °C

실험 절차

50 g of 2-methoxycarbonylamino-5,6-dimethoxy-1-tetralone are dissolved in 500 ml of methanol in a 1000 ml flask, with stirring, 20 g of 5% Pd/C are added, then the whole is placed into an autoclave (Hastelloy) under hydrogen atmosphere at 80° C. and a pressure of 25 atm. for about 6 hours with stirring, after that the mixture is left to cool to about 30° C. in autoclave. The mixture is filtered through Celite and the filtrate is evaporated to dryness under vacuum. The resulting white solid is triturated in 400 ml of n-hexane at 60° C., then is left to cool to about 30° C. with stirring, filtered and dried under vacuum at 60 ° C., to obtain a whitish solid. Yield: 40.6 g, 85.5% (moles), 81.2% (weight); T.L.C. Methylene chloride 95-Methanol 5; Rf=0.76; M.p.=108.7°-111.4 ° C.

후처리

  1. stirringa pressure of 25 atm. for about 6 hours with stirring
  2. waitafter that the mixture is left
  3. filtrationThe mixture is filtered through Celite
  4. customthe filtrate is evaporated to dryness under vacuum
  5. customThe resulting white solid is triturated in 400 ml of n-hexane at 60° C.
  6. waitis left
  7. temperatureto cool to about 30° C.
  8. stirringwith stirring
  9. filtrationfiltered
  10. customdried under vacuum at 60 ° C.
  11. customto obtain a whitish solid

출처 및 근거

ORD 기록
ord-060cf77c801f4c2b9ab5e12da8b48f29
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05710336

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