Acetic Anhydride → HCID 178526759、化合物

HRID 1670469ノート

反応式

HRID 1670469 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

実験手順

29 g (101 mmol) of 5-bromo-2-(2-nitro-vinylamino)-benzoic acid (Example 1a) and 11.9 g (121 mmol) of potassium acetate in 129 ml (152 mmol) of acetic anhydride are stirred for 1.5 h at 120° C. The precipitate is filtered off and washed with acetic acid until the filtrate is colorless, then is washed with H2O and dried in vacuo to give the title compound. ES-MS: 269, 271 (M+H)+, Br pattern; analytical HPLC: tret=2.70 min (Grad 1).

後処理

  1. filtrationThe precipitate is filtered off
  2. washwashed with acetic acid until the filtrate
  3. washis washed with H2O
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-f72709ca45c3460481c6b6e2e46fe5e7
出典データセット
uspto-grants-2011_08
特許番号
US07994170B2

反応ノート

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