Sodium Perborate → HCID 59438049, Verbindung

HRID 474209Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 474209
B(O[O-])=[O:2].[Na+].[CH3:6][N:7]1[CH:11]=[C:10]([C:12]2[CH:13]=[CH:14][C:15](=[O:40])[N:16]([CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([C:25]4[N:30]=[CH:29][C:28](B5OC(C)(C)C(C)(C)O5)=[CH:27][N:26]=4)[CH:20]=3)[N:17]=2)[CH:9]=[N:8]1>C1COCC1.O>[OH:2][C:28]1[CH:27]=[N:26][C:25]([C:21]2[CH:20]=[C:19]([CH:24]=[CH:23][CH:22]=2)[CH2:18][N:16]2[C:15](=[O:40])[CH:14]=[CH:13][C:12]([C:10]3[CH:9]=[N:8][N:7]([CH3:6])[CH:11]=3)=[N:17]2)=[N:30][CH:29]=1

Komponenten

5

Edukt 2

HCID 517072Sodium PerborateHCID 594380506-(1-Methyl-1H-pyrazol-4-yl)-2-[[3-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-pyrimidinyl]phenyl]methyl]-3(2H)-pyridazinone

Produkt 1

HCID 59438049HCID 59438049, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

8.50 g (85.1 mmol) of sodium perborate are added in portions with ice-cooling to a suspension of 13.4 g (28.4 mmol) of 6-(1-methyl-1H-pyrazol-4-yl)-2-{3-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-yl]benzyl}-2H-pyridazin-3-one in 55 ml of THF and 55 ml of water, and the mixture is stirred at room temperature for 2 hours. The reaction mixture is filtered off through kieselguhr with suction. The filtrate is evaporated to about half of the original volume in vacuo and adjusted to a pH of 1 using 2 N hydrochloric acid. The precipitate formed is filtered off with suction, washed with water and dried in vacuo: 2-[3-(5-hydroxypyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one as pale-beige crystals; m.p. 239° C.; ESI 361.

Aufarbeitung

  1. filtrationThe reaction mixture is filtered off through kieselguhr with suction
  2. customThe filtrate is evaporated to about half of the original volume in vacuo
  3. customThe precipitate formed
  4. filtrationis filtered off with suction
  5. washwashed with water
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-fc59402665964bd6a1992845b4812b92
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08637518B2

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