Water → HCID 18005159, Verbindung

HRID 1603782Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1603782
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]2[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=2)[C:7]2[O:11][CH2:10][CH2:9][C:8]=2[CH:12]=1)([O-])=O.[Sn].O.[OH-].[Na+]>C(O)C.Cl>[NH2:1][C:4]1[CH:5]=[C:6]([C:13]2[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=2)[C:7]2[O:11][CH2:10][CH2:9][C:8]=2[CH:12]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 5352426Tin atom2×HCID 18005129HCID 18005129, Verbindung

Produkt 1

HCID 18005159HCID 18005159, VerbindungAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel2×HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

2,3-Dihydro-5-nitro-7-(pyrid-3-yl)benzofuran (D63) (0.19 g, 0.00079 mole) in ethanol (20 ml) was treated with a solution of tin II chloride (0.75 g, 0.0040 mole) in conc. hydrochloric acid (1 ml) and heated at 50° C. for 2 hours. A further 0.38 g tin II chloride in conc. hydrochloric acid (0.5 ml) was added and the mixture was heated at 50° C. for 1/2 hour and stirred at ambient temperature for 18 hours. Deionised water (5 ml) was added and the mixture was basified with 10% sodium hydroxide solution, extracted into ethyl acetate, dried (Na2SO4) and evaporated in vacuo to afford the title compound (0.13 g, 82%) as a dark oil.

Aufarbeitung

  1. temperaturethe mixture was heated at 50° C. for 1/2 hour
  2. extractionextracted into ethyl acetate
  3. dry with materialdried (Na2SO4)
  4. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d7ccdcb939364f50a3240b656c8f0f42
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05990133

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