Isopropanol → HCID 23717654, Verbindung

HRID 1413803Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1413803
C[O-].[Na+:3].[F:4][C:5]1[CH:26]=[C:25]([Br:27])[CH:24]=[CH:23][C:6]=1[CH2:7][N:8]1[N:17]=[C:16]([CH2:18][C:19]([OH:21])=[O:20])[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]1=[O:22].C(O)(C)C>CO>[F:4][C:5]1[CH:26]=[C:25]([Br:27])[CH:24]=[CH:23][C:6]=1[CH2:7][N:8]1[N:17]=[C:16]([CH2:18][C:19]([O-:21])=[O:20])[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]1=[O:22].[Na+:3]

Komponenten

5

Edukt 3

HCID 3776IsopropanolHCID 5278PonalrestatHCID 10942334Sodium Methoxide

Produkt 1

HCID 23717654HCID 23717654, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel3×

Versuchsvorschrift

A solution of sodium methoxide (25 ml. of a 1.0 M solution in methanol) was added to a solution of 2-(2-fluoro-4-bromobenzyl)-1,2-dihydro-1-oxophthalazin-4-ylacetic acid (9.87 g.) in methanol (300 ml.) and the mixture heated to its boling point. Methanol was then allowed to boil off until the volume of the mixture was approximately 100 ml. Isopropanol (150 ml.) was then added, followed by petrol (60-80) until the mixture was just opaque. The mixture was then allowed to cool to room temperature. The solid which formed was separated by filtration, evaporated with toluene (2×400 ml.) and then washed with ether (300 ml.) to give sodium 2-(2-fluoro-4-bromobenzyl)-1,2-dihydro-1-oxophthalazin-4-ylacetate, 6.5 g., m.p. 244°-247° C.

Aufarbeitung

  1. temperaturethe mixture heated to its boling point
  2. customThe solid which formed
  3. customwas separated by filtration
  4. customevaporated with toluene (2×400 ml.)
  5. washwashed with ether (300 ml.)

Quellen und Nachweise

ORD-Eintrag
ord-9942c679acaf4ffeae8a07242c621f5b
Quelldatensatz
uspto-grants-1981_02
Patentnummer
US04251528

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