Acetic Acid → HCID 69043799, Verbindung

HRID 1894907Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1894907
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][C:9](=[O:20])[C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)=[CH:4][C:3]=1[C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([N+:27]([O-])=O)[CH:22]=1.C(O)(=O)C.C([O-])([O-])=O.[Na+].[Na+]>C(O)C.[Fe]>[NH2:27][C:23]1[CH:22]=[C:21]([C:3]2[CH:4]=[C:5]([NH:8][C:9](=[O:20])[C:10]3[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:17])[F:18])[CH:11]=3)[CH:6]=[N:7][C:2]=2[CH3:1])[CH:26]=[CH:25][CH:24]=1

Komponenten

6

Reaktionsbedingungen

Temperatur
87 °C

Versuchsvorschrift

To a solution of N-[6-methyl-5-(3-nitrophenyl)pyridin-3-yl]-3-(trifluoromethyl)benzamide (0.150 g, 0.000374 mol) in ethanol (3 mL) was added acetic acid (0.5 mL, 0.009 mol) and iron powder (0.11 g, 0.0020 mol). The reaction was heated at 87° C. for 2 hours. It was then neutralized with Na2CO3 and extracted with EtOAc and the organic extracts were washed with water, saturated NaCl, dried (MgSO4) and stripped in vacuo. The residue was used in the next reaction without purification. MS (ES) (M+H)=372.

Aufarbeitung

  1. extractionextracted with EtOAc
  2. washthe organic extracts were washed with water, saturated NaCl
  3. dry with materialdried (MgSO4)
  4. customThe residue was used in the next reaction without purification

Quellen und Nachweise

ORD-Eintrag
ord-79d0a065087f4384a23b137a3ea35f16
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08513270B2

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