Hydrogen Bromide → HCID 19850133, Verbindung

HRID 1608010Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1608010
Cl.Cl.[F:3][C:4]1[CH:5]=[C:6]([CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:7]=[CH:8][C:9]=1[O:10]C.[BrH:30]>[PH2](O)=O>[BrH:30].[BrH:30].[F:3][C:4]1[CH:5]=[C:6]([CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:7]=[CH:8][C:9]=1[OH:10]

Komponenten

4

Edukt 2

HCID 260Hydrogen BromideHCID 19850140HCID 19850140, Verbindung

Produkt 1

HCID 19850133HCID 19850133, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 4124402Phosphinic AcidKatalysator

Versuchsvorschrift

The product from step (b) (1.8 g) in 48% hydrobromic acid (18 ml) containing hypophosphorous acid (10 drops) was boiled at reflux under nitrogen for 5.5 hr. The solid which separated on cooling the solution was collected and recrystallised from water giving the dihydrobromide salt of the title compound as colourless needles (1.3 g) mp 240.5-142°-5°.

Aufarbeitung

  1. temperatureat reflux under nitrogen for 5.5 hr
  2. customThe solid which separated
  3. temperatureon cooling the solution
  4. customwas collected
  5. customrecrystallised from water giving the dihydrobromide salt of the title compound as colourless needles (1.3 g) mp 240.5-142°-5°

Quellen und Nachweise

ORD-Eintrag
ord-78bf1d0580234c5da4a121c0d370a381
Quelldatensatz
uspto-grants-1989_09
Patentnummer
US04868306

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