Hydrochloric Acid → HCID 21249960, Verbindung

HRID 1531653Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1531653
Cl.[BH4-].[Na+].[Br:4][C:5]1[C:6]([O:26][CH3:27])=[CH:7][C:8]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=3)=[N:13][N:12]=[C:11]([CH3:24])[CH2:10][C:9]=2[CH:25]=1>CO.O>[Br:4][C:5]1[C:6]([O:26][CH3:27])=[CH:7][C:8]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=3)=[N:13][NH:12][CH:11]([CH3:24])[CH2:10][C:9]=2[CH:25]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 21249973HCID 21249973, Verbindung

Produkt 1

HCID 21249960HCID 21249960, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

3.5 ml (43.2 mmol) of concentrated hydrochloric acid is first added, and then over about 10 minutes, 1.80 g (47.5 mmol) of sodium borohydride is added in portions to a suspension of 1.4 g (3.6 mmol) of 7-bromo-4-methyl-8-methoxy-1-(4-nitrophenyl)-5H-2,3-benzodiazepine (Example 3, Step C) in 60 ml of methanol. The suspension is stirred for another hour, and then diluted with water (60 ml). The crystalline material is suctioned off and washed with 50% aqueous methanol (3×50 ml). The 7-bromo-4-methyl-8-methoxy-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine that is obtained as a crude product is further purified by suspension in 8 ml of hot ethanol. After suctioning-off, 1.23 g (88%) of chrome yellow crystals with a melting point of 172-174° C. is obtained.

Aufarbeitung

  1. washwashed with 50% aqueous methanol (3×50 ml)

Quellen und Nachweise

ORD-Eintrag
ord-d3cd79cfa23c4dbaabf64448cfb7e33c
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06200970B1

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