Nitric Acid → HCID 131728508, Verbindung

HRID 2425087Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2425087
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([CH3:21])[C:8]2[O:14][C:13]3[C:15]([Cl:19])=[CH:16][CH:17]=[CH:18][C:12]=3[CH2:11][S:10][C:9]=2[CH:20]=1)=[O:4].[N+:22]([O-])([OH:24])=[O:23].S(=O)(=O)(O)[OH:27]>>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([CH3:21])[C:8]2[O:14][C:13]3[C:15]([Cl:19])=[CH:16][C:17]([N+:22]([O-:24])=[O:23])=[CH:18][C:12]=3[CH2:11][S:10](=[O:27])[C:9]=2[CH:20]=1)=[O:4]

Komponenten

4

Versuchsvorschrift

Compound of Example 15b (4.1 g, 12.8 mmol) was added to solution of nitrating mixture (nitric acid 200 mL and sulfuric acid 20 mL) at 0° C. and stirred for 18 h. The reaction mixture was poured slowly with stirring into ice water (200 mL). The solid separated was filtered, washed with water and dried to obtain the title compound. Yield: 2.5 g, (52%); 1H NMR (CDCl3, 300 MHz): δ 2.65 (s, 3H, CH3), 3.93 (s, 3H, OCH3), 4.57 (s, 2H, CH2), 8.16 (d, 2H, Ar), 8.35 (d, 2H, Ar); MS: m/e (ES−) 380 (M−1).

Aufarbeitung

  1. additionThe reaction mixture was poured slowly
  2. customThe solid separated
  3. filtrationwas filtered
  4. washwashed with water
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c0eefcb999d641e7a83fe6b08ec93bf0
Quelldatensatz
uspto-grants-2011_06
Patentnummer
US07964631B2

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