HCID 67100256, Verbindung → HCID 57983375, Verbindung

HRID 1868805Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1868805
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:10]=2)[C:5]2([CH2:21][CH2:20][CH2:19][CH2:18]2)[C:4](=[O:22])[C:3]=1[C:23]([NH:25][CH2:26][C:27]([O:29]C(C)(C)C)=[O:28])=[O:24]>C(O)(C(F)(F)F)=O.CCOCC>[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:10]=2)[C:5]2([CH2:21][CH2:20][CH2:19][CH2:18]2)[C:4](=[O:22])[C:3]=1[C:23]([NH:25][CH2:26][C:27]([OH:29])=[O:28])=[O:24]

Komponenten

4

Edukt 1

HCID 67100256HCID 67100256, Verbindung

Produkt 1

HCID 57983375HCID 57983375, VerbindungAusbeute 20,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

1,1-Dimethylethyl N-((4′-hydroxy-2′-oxo-6′-phenyl-spiro[cyclopentane-1,1′-naphthalen]-3′-yl)carbonyl)glycinate (115 mg, 257 μmol) was dissolved in TFA (2 mL) at ambient temperature. The reaction was stirred for 30 minutes and was then concentrated to give an oil, dissolved in ether, concentrated again to give an amorphous solid, precipitated with ether, filtered, washed with ether, and dried in a vacuum oven to give the title compound (21 mg) as a white solid. MS (m/z)=392 (M+H)+. Calculated for the C23H21NO5 391.14.

Aufarbeitung

  1. concentrationwas then concentrated
  2. customto give an oil
  3. concentrationconcentrated again
  4. customto give an amorphous solid
  5. customprecipitated with ether
  6. filtrationfiltered
  7. washwashed with ether
  8. customdried in a vacuum oven

Quellen und Nachweise

ORD-Eintrag
ord-d1de8b80a5274a2d9e9f7b388625b10e
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07635715B2

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