Acetic Acid → 2-Iodo-4-nitrobenzoic acid

HRID 968278

反応式

HRID 968278 の反応式
[I-].[K+].[I:3]([C:5]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8])=O.C(O)(=O)C>O>[I:3][C:5]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[CH:10][C:6]=1[C:7]([OH:9])=[O:8]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 4875Potassium IodideHCID 3714830Benzoic acid, 2-iodosyl-4-nitro-

生成物 1

HCID 4589642-Iodo-4-nitrobenzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
23 °C

実験手順

Solid potassium iodide (55 g, 0.33 mol) was added in one portion to a suspension of 2-iodosyl-4-nitro-benzoic acid I-1a (54.9 g, 0.18 mol) in water (250 ml) and glacial acetic acid (50 ml). Over the next 5-10 minutes, the solids gradually went into solution and the solution turned from off-white to red. After stirring for one hour at 23° C., gaseous sulfur dioxide was bubbled through the reaction mixture until the red color dissipated and a pale green suspension had formed. The solids were collected by filtration, co-evaporated from toluene (3×250 ml), and dried in vacuo to affort 2-iodo-4-nitrobenzoic acid I-1b (33 g, 64%).

後処理

  1. customOver the next 5-10 minutes
  2. customgaseous sulfur dioxide was bubbled through the reaction mixture until the red color
  3. customa pale green suspension had formed
  4. filtrationThe solids were collected by filtration
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-3c96c164c96c4e5680b852debc230534
出典データセット
uspto-grants-2005_10
特許番号
US06958347B2

関連ノート

読み込み中…