Nitric Acid → HCID 131728508, Verbindung

HRID 1173356Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1173356
[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

Edukt 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 672474734-Chloro-6-methyl-11h-5-oxa-10-thia-dibenzo[a,d]cycloheptene-8-carboxylic acid methyl ester

Produkt 1

HCID 131728508HCID 131728508, Verbindung

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-eccd75b8db494727a0d1f51c099a7f30
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07834052B2

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