Ammonia → HCID 67263977, Verbindung

HRID 1041059Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1041059
[CH3:1][O:2][C:3]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:6]2[N:7]([CH3:19])[C:8](=[O:18])[CH2:9][N:10](C(=O)C(F)(F)F)[CH2:11][C:5]=2[CH:4]=1.N>CO>[CH3:1][O:2][C:3]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][C:6]2[N:7]([CH3:19])[C:8](=[O:18])[CH2:9][NH:10][CH2:11][C:5]=2[CH:4]=1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 86633916HCID 86633916, Verbindung

Produkt 1

HCID 67263977HCID 67263977, VerbindungAusbeute 77,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 7-Methoxy-1-methyl-8-nitro-4-(2,2,2-trifluoro-acetyl)-1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one (2.86 g, 0.00824 mol) and 7.0 M of Ammonia in Methanol (30 mL) were reacted in an analogous manner to example 736-D to give an oil. 7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro[e][1,4]diazepin-2-one It was triturated with diethyl ether giving 7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro-benzo[e][1,4]diazepin-2-one as a tan solid (1.61 g, 77%). Mp145-149° C.; LCMS (m/e) 252 (M+1); 1H-NMR (DMSO, 400 MHz) δ 7.91 (s, 1H), 7.41 (s, 1H), 3.94 (s, 2H), 3.79 (s, 1H), 3.31 (s, 3H), 3.25 (s, 2H).

Aufarbeitung

  1. customwere reacted in an analogous manner to example 736-D
  2. customto give an oil
  3. custom7-Methoxy-1-methyl-8-nitro-1,3,4,5-tetrahydro[e][1,4]diazepin-2-one It was triturated with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-0f22f65e4a5249188e085d6ea91eba0b
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08552186B2

Notizen zur Reaktion

Wird geladen…