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Perchloric Acid → HCID 67181870, Verbindung

HRID 2410417
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2410417
Cl(O)(=O)(=O)=O.[CH3:6][O:7][C:8]1[N:13]=[CH:12][C:11]([C:14]2[CH:19]=[CH:18][C:17]([CH2:20][CH2:21][C@H:22]3[O:31][C@H:25]4[O:26]C(C)(C)[O:28][C@H:24]4[C@H:23]3[CH2:32][CH2:33][N:34]3[C:42](=[O:43])[C:41]4[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=4)[C:35]3=[O:44])=[CH:16][CH:15]=2)=[CH:10][CH:9]=1>C(#N)C.C(OCC)(=O)C.O>[OH:28][C@@H:24]1[C@H:25]([OH:26])[O:31][C@H:22]([CH2:21][CH2:20][C:17]2[CH:18]=[CH:19][C:14]([C:11]3[CH:12]=[N:13][C:8]([O:7][CH3:6])=[CH:9][CH:10]=3)=[CH:15][CH:16]=2)[C@@H:23]1[CH2:32][CH2:33][N:34]1[C:35](=[O:44])[C:36]2[C:41](=[CH:40][CH:39]=[CH:38][CH:37]=2)[C:42]1=[O:43]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 24247Perchloric AcidHCID 671812512-{2-[(3aS,5R,6S,6aS)-5-{2-[4-(6-methoxypyridin-3-yl)phenyl]ethyl}-2,2-dimethyltetrahydrofuro[2,3-d][1,3]dioxol-6-yl]ethyl}-1H-isoindole-1,3(2H)-dione

Produkt 1

HCID 67181870HCID 67181870, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×
HCID 6342
Acetonitrile
Lösungsmittel
HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

Perchloric acid (0.4 mL) was added to a solution of the compound obtained from step f above (0.5 g) in acetonitrile (4 mL) and water (0.8 mL) at room temperature. The reaction mixture was heated to 55° C. for 30 minutes. The reaction mixture was then quenched using sodium bicarbonate solution. The solvents were evaporated under reduced pressure. The residue thus obtained was taken up in ethyl acetate and water. The organic layer was separated, washed with water and brine solution, and dried over anhydrous sodium sulphate. The solvent was concentrated under reduced pressure to yield the title compound (0.51 g).

Aufarbeitung

  1. customat room temperature
  2. customThe reaction mixture was then quenched
  3. customThe solvents were evaporated under reduced pressure
  4. customThe residue thus obtained
  5. customThe organic layer was separated
  6. washwashed with water and brine solution
  7. dry with materialdried over anhydrous sodium sulphate
  8. concentrationThe solvent was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-23b9a9f9fb29489fb6a2e432078ee471
Quelldatensatz
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08816073B2

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