Acetic Anhydride → Acetamide, N-[4-fluoro-3-(trifluoromethyl)phenyl]-

HRID 54375

Reaktionsgleichung

Reaktionsgleichung von HRID 54375
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]([F:12])([F:11])[F:10])[C:5]([F:8])=[CH:6][CH:7]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14]>CCN(CC)CC>[C:13]([NH:1][C:2]1[CH:3]=[C:4]([C:9]([F:12])([F:10])[F:11])[C:5]([F:8])=[CH:6][CH:7]=1)(=[O:15])[CH3:14]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 753774-Fluoro-3-(trifluoromethyl)aniline

Produkt 1

HCID 10353438Acetamide, N-[4-fluoro-3-(trifluoromethyl)phenyl]-Ausbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

A solution of 3-amino-6-fluorobenzotrifluoride (2.0 g, 11.17 mmol, Aldrich) in acetic anhydride (10 mL) and Et3N (1 mL) was stirred at room temperature for 24 h, and then most of the acetic anhydride was removed. The white needle crystals were collected by filtration and washed with water (2×2 mL), affording 2.4 g (97%) of 3-acetamido-6-fluorobenzotrifluoride. 1H NMR (CDCl3): δ2.184 (s, 3H); 7.136 (t, 1H, J=9.9 Hz); 7.733 (m, 3H).

Aufarbeitung

  1. custommost of the acetic anhydride was removed
  2. filtrationThe white needle crystals were collected by filtration
  3. washwashed with water (2×2 mL)

Quellen und Nachweise

ORD-Eintrag
ord-890b39580f944ef89398cbf59463adc2
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05622952

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