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2-Indanone → 1020634-41-6

HRID 2278702
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2278702
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[N:8]([CH2:12][CH3:13])[CH:7]=[C:6]([C:14]([O:16]CC)=O)[C:5]2=[O:19].[CH2:20]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22][C:21]1=O.[B].[OH-:31].[Na+]>C(OCC)(=O)C.C(O)(=O)C>[CH2:20]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22][CH:21]1[NH:1][C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[N:8]([CH2:12][CH3:13])[CH:7]=[C:6]([C:14]([N:8]1[CH2:9][CH2:4][O:31][CH2:6][CH2:7]1)=[O:16])[C:5]2=[O:19]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 119832-IndanoneHCID 14798Sodium HydroxideHCID 5462311BoronHCID 59293371HCID 59293371, Verbindung

Produkt 1

HCID 247721651020634-41-6

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittel
HCID 8857
Ethyl Acetate
Lösungsmittel

Reaktionsbedingungen

Temperatur
42.5 °C

Versuchsvorschrift

Other Alternative Methods. To a suspension of ethyl 6-amino-1-ethyl-4-oxo-1,8-naphthyridine-3-carboxylate in a solvent specified in Table 1 was added acetic acid and the mixture was stirred until all solids went into solution (may need to warm up to 40-45° C.). 2-Indanone was added to reaction mixture and stirred to completion of imine formation (indicated by disappearance of starting material in LCMS) (˜30 min to 1 h). Boron reducing agent (as listed in Table 1) was added to reaction mixture and stirred vigorously to completion of imine reduction (disappearance of imine in LCMS). The reaction mixture was transferred to a beaker, diluted with ethyl acetate, added an ice-cooled aqueous sodium hydroxide solution (1.0 M) (enough to quench almost 90% of acetic acid) and then further basified with solid sodium bicarbonate to pH 7-8. The organic layer was separated, washed with brine, dried over MgSO4 and evaporated under reduced pressure to dryness. Where specified in Table 1, the crude was passed through a plug of silica gel with increasing gradient of EtOAc in DCM to offer the required product as dark yellow solid.

Aufarbeitung

  1. customto quench almost 90% of acetic acid) and
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. customevaporated under reduced pressure to dryness
  6. temperaturewith increasing gradient of EtOAc in DCM

Quellen und Nachweise

ORD-Eintrag
ord-8d36ad3d1de7471290ca425a986a0387
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09133188B2

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