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

HRID 54375ノート

反応式

HRID 54375 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-890b39580f944ef89398cbf59463adc2
出典データセット
uspto-grants-1997_04
特許番号
US05622952

反応ノート

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