Ammonia → 4-(Aminomethyl)-2-methoxybenzonitrile

HRID 1278926Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1278926
Br[CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[C:5]([O:11][CH3:12])[CH:4]=1.CO.[NH3:15].N.CO>C(Cl)Cl>[NH2:15][CH2:2][C:3]1[CH:10]=[CH:9][C:6]([C:7]#[N:8])=[C:5]([O:11][CH3:12])[CH:4]=1

Komponenten

6

Versuchsvorschrift

2.5 g of the bromide (b) were introduced into 10 ml of MeOH, and NH3 was passed in during dropwise addition of 38 ml of conc. ammonia/MeOH 1:1. After 2 h, the solvent was stripped off, the product was taken up in DCM and washed with water, and the organic phase was dried over Na2SO4. The product was precipitated as hydrochloride with ethereal HCl. 1H-NMR (DMSO-d6, δ in ppm): 8.6 (broad signal, NH3+), 7.79 (1H), 7.55 (1H), 7.20 (1H), 4.10 (s, 2H), 3.93 (s, 3H)

Aufarbeitung

  1. washwashed with water
  2. dry with materialthe organic phase was dried over Na2SO4
  3. customThe product was precipitated as hydrochloride with ethereal HCl

Quellen und Nachweise

ORD-Eintrag
ord-9d67b28124344561a17a4f48759d32e0
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06444817B1

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