Sodium Hydroxide → HCID 20324952, Verbindung

HRID 838855Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 838855
[CH2:1]([C:5]1[CH:10]=[C:9]([CH2:11][CH2:12][CH2:13][CH3:14])[N:8]2[N:15]=[CH:16][CH:17]=[C:7]2[N:6]=1)[CH2:2][CH2:3][CH3:4].[Br:18]N1C(=O)CCC1=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[Br:18][C:17]1[CH:16]=[N:15][N:8]2[C:9]([CH2:11][CH2:12][CH2:13][CH3:14])=[CH:10][C:5]([CH2:1][CH2:2][CH2:3][CH3:4])=[N:6][C:7]=12

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 67184N-bromobutanimideHCID 203249445,7-Dibutylpyrazolo[1,5-a]pyrimidine

Produkt 1

HCID 20324952HCID 20324952, VerbindungAusbeute 76,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A solution of 7.0 g (0.03 mol) of 5,7-di-n-butylpyrazolo[1,5-a]-pyrimidine in 75 ml chloroform was treated with 5.8 g (0.035 mol) of N-bromosuccinimide at room temperature. The mixture was stirred for 5-10 minutes, then poured into ice water, made alkaline with 6N NaOH, and the organic layer separated and dried (Na2SO4). The chloroform solution was chromatographed on neutral alumina (Woelm, grade I) with chloroform as the eluant. Evaporation of the solvent and recrystallization from ligroine gave 7.15 g (72%) of the product, mp 47°-48° C.

Aufarbeitung

  1. customthe organic layer separated
  2. dry with materialdried (Na2SO4)
  3. customThe chloroform solution was chromatographed on neutral alumina (Woelm, grade I) with chloroform as the eluant
  4. customEvaporation of the solvent and recrystallization from ligroine

Quellen und Nachweise

ORD-Eintrag
ord-97b69ec5311349f7bc3f44710ecb64a4
Quelldatensatz
uspto-grants-1978_06
Patentnummer
US04093617

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