Sulfuric Acid → Benzoic acid, 2-iodosyl-4-nitro-

HRID 968277

반응식

HRID 968277 반응식
[I:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4]C=1C.C([O:15][C:16](=[O:18])[CH3:17])(=O)C.S(=O)(=O)(O)[OH:20]>[O-2].[O-2].[O-2].[Cr+6].C(O)(=O)C>[I:1]([C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:17]=1[C:16]([OH:15])=[O:18])=[O:20]

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 821882-Iodo-4-nitrotoluene

생성물 1

HCID 3714830Benzoic acid, 2-iodosyl-4-nitro-

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 176Acetic Acid용매

실험 절차

A solution of 2-iodo-4-nitrotoluene (50 g, 0.19 mol) in a mixture of glacial acetic acid (380 ml), acetic anhydride (190 ml) and concentrated sulfuric acid (112 ml) was cooled in an ice bath. Chromium trioxide (97 g, 0.57 mol) was added portionwise over 30 minutes, during which time the internal temperature rose to ca. 90° C. The resultant thick suspension was cooled in an ice bath for 30 min, then poured over ice (2 kg). When the ice had melted, the precipitate was collected by filtration, washed with methanol (800 ml) and ether (200 ml), and dried in vacuo to afford 2-iodosyl-4-nitro-benzoic acid I-1a (54.9 a, 94%).

후처리

  1. temperaturewas cooled in an ice bath
  2. customrose to ca. 90° C
  3. temperatureThe resultant thick suspension was cooled in an ice bath for 30 min
  4. filtrationthe precipitate was collected by filtration
  5. washwashed with methanol (800 ml) and ether (200 ml)
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-76a1c87a39a647bea16b3b39d661fe60
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06958347B2

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