HCID 67100256, Verbindung → HCID 57983375, Verbindung

HRID 2078213Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2078213
[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-8756e05bde4e4c198ecf2db6c31bc20d
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928139B2

Notizen zur Reaktion

Wird geladen…