Glutaric anhydride → 5-(4-[(4aS,8aR)-4-(3,4-Diethoxy-phenyl)-1-oxo-4a,5,8,8a-tetrahydro-1H-phthalazin-2-yl]-piperidin-1-yl)-5-oxo-pentanoic Acid

HRID 967312Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 967312
[C:1]1(=[O:8])[O:7][C:5](=[O:6])[CH2:4][CH2:3][CH2:2]1.[CH2:9]([O:11][C:12]1[CH:13]=[C:14]([C:21]2[C@@H:30]3[C@@H:25]([CH2:26][CH:27]=[CH:28][CH2:29]3)[C:24](=[O:31])[N:23]([CH:32]3[CH2:37][CH2:36][N:35](S(C4C=CC(C)=CC=4)(=O)=O)[CH2:34][CH2:33]3)[N:22]=2)[CH:15]=[CH:16][C:17]=1[O:18][CH2:19][CH3:20])[CH3:10]>>[CH2:9]([O:11][C:12]1[CH:13]=[C:14]([C:21]2[C@@H:30]3[C@@H:25]([CH2:26][CH:27]=[CH:28][CH2:29]3)[C:24](=[O:31])[N:23]([CH:32]3[CH2:33][CH2:34][N:35]([C:5](=[O:6])[CH2:4][CH2:3][CH2:2][C:1]([OH:7])=[O:8])[CH2:36][CH2:37]3)[N:22]=2)[CH:15]=[CH:16][C:17]=1[O:18][CH2:19][CH3:20])[CH3:10]

Komponenten

3

Edukt 2

HCID 7940Glutaric anhydrideHCID 10175016(4aS,8aR)-4-(3,4-Diethoxyphenyl)-2-[1-(toluene-4-sulfonyl)-piperidin-4-yl]-4a,5,8,8a-tetrahydro-2H-phthalazin-1-one

Produkt 1

HCID 101960635-(4-[(4aS,8aR)-4-(3,4-Diethoxy-phenyl)-1-oxo-4a,5,8,8a-tetrahydro-1H-phthalazin-2-yl]-piperidin-1-yl)-5-oxo-pentanoic Acid

Versuchsvorschrift

Prepared from glutaric anhydride and starting compound A2 as described for compound 1. After evaporating the pyridine, the residue is partitioned between ethyl acetate and 1N hydrochloric acid. The ethyl acetate solution is dried over magnesium sulfate and evaporated. Crystallisation from diethyl ether. M. p. 133-135° C.

Aufarbeitung

  1. customAfter evaporating the pyridine
  2. customthe residue is partitioned between ethyl acetate and 1N hydrochloric acid
  3. dry with materialThe ethyl acetate solution is dried over magnesium sulfate
  4. customevaporated
  5. customCrystallisation from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-aa14bee00c2d41e4aef49e9d938faaad
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06953853B2

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