Acetic Acid → 2-Iodo-4-nitrobenzoic acid

HRID 968278

반응식

HRID 968278 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 4589642-Iodo-4-nitrobenzoic acid

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
23 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3c96c164c96c4e5680b852debc230534
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06958347B2

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