Acetic Anhydride → HCID 178526759、化合物

HRID 2174937ノート

反応式

HRID 2174937 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:11][CH:12]=[CH:13][N+:14]([O-:16])=[O:15])=[C:6]([CH:10]=1)[C:7](O)=[O:8].C([O-])(=O)C.[K+].C(OC(=O)C)(=O)C>>[Br:1][C:2]1[CH:10]=[C:6]2[C:5](=[CH:4][CH:3]=1)[N:11]=[CH:12][C:13]([N+:14]([O-:16])=[O:15])=[C:7]2[OH:8]

参加物

4

反応物 3

HCID 7918Acetic AnhydrideHCID 517044Potassium AcetateHCID 534050555-Bromo-2-(2-nitrovinylamino)benzoic acid2 回

生成物 1

HCID 178526759HCID 178526759、化合物

実験手順

5-Bromo-2-(2-nitrovinylamino)benzoic acid (Compound A, 87 mmol) and potassium acetate (104 mmol) in acetic anhydride (1185 mmol) were stirred for 3 h at 120° C. The precipitate was filtered, and washed with acetic acid till the filtrate was colorless. It was further washed with water and dried to obtain the title compound. 1H NMR (CDCl3, 500 MHz): δ 9.275 (s, 1H), 8.611-8.615 (d, 1H, J=2 Hz), 8.100-8.118 (d, 1H, J=9 Hz), 8.026-8.048 (dd, 1H, J=8.5 Hz, 2 Hz).

後処理

  1. filtrationThe precipitate was filtered
  2. washwashed with acetic acid till the filtrate
  3. washIt was further washed with water
  4. customdried

出典と根拠

ORDレコード
ord-6a47060f17eb4b72bd7cefedc29090b8
出典データセット
uspto-grants-2015_06
特許番号
US09062046B2

反応ノート

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