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HCID 19898936, 화합물 → HCID 19898935, 화합물

HRID 1607121
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HRID 1607121 반응식
C([N:8]([C:13]1[CH:18]=[CH:17][C:16]([CH:19]([OH:36])[CH2:20][N:21]([CH2:23][CH2:24][N:25]2[N:34]=[CH:33][C:32]3[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=3)[C:26]2=[O:35])[CH3:22])=[CH:15][CH:14]=1)[S:9]([CH3:12])(=[O:11])=[O:10])C1C=CC=CC=1>C(O)C.C(OCC)C.[Pd]>[CH3:12][S:9]([NH:8][C:13]1[CH:18]=[CH:17][C:16]([CH:19]([OH:36])[CH2:20][N:21]([CH2:23][CH2:24][N:25]2[N:34]=[CH:33][C:32]3[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=3)[C:26]2=[O:35])[CH3:22])=[CH:15][CH:14]=1)(=[O:10])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 19898936HCID 19898936, 화합물

생성물 1

HCID 19898935HCID 19898935, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

N-[2-(4-{N-Benzylmethanesulphonamido}phenyl)-2-hydroxyethyl]-N-methyl-2-(phthalazin-1-on-2-yl)ethylamine (0.4 g--as solvate from part D) in ethanol (50 ml) containing 5% Pd/C (0.1 g) was stirred under a hydrogen atmosphere (50 p.s.i.) at 50° for 18 hours. The reaction mixture was then filtered and the ethanol removed. The residue was dissolved in methylene chloride and washed three times with sodium bicarbonate solution and three times with brine. The organic layer was dried and evaporated to give an oil which was purified by column chromatography on silica, "Kieselgel 60" (Merck, Trade Mark), eluting with methylene chloride containing methanol (0% up to 2%). The appropriate fractions were combined and evaporated to give an oil which solidified after stirring for 14 hours in diethyl ether, filtration giving the title compound, 0.11 g, m.p. 134°-137°.

후처리

  1. filtrationThe reaction mixture was then filtered
  2. customthe ethanol removed
  3. dissolutionThe residue was dissolved in methylene chloride
  4. washwashed three times with sodium bicarbonate solution and three times with brine
  5. customThe organic layer was dried
  6. customevaporated
  7. customto give an oil which
  8. customwas purified by column chromatography on silica, "Kieselgel 60" (Merck, Trade Mark)
  9. washeluting with methylene chloride
  10. additioncontaining methanol (0% up to 2%)
  11. customevaporated
  12. customto give an oil which
  13. filtrationfiltration

출처 및 근거

ORD 기록
ord-7d1235c757a14feaa86ee208b2e5420d
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04863948

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