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Sulfuric Acid → HCID 22457397, 화합물

HRID 2184630
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HRID 2184630 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([OH:15])=[O:14])[C:7](=[CH:11][CH:12]=1)[C:8]([OH:10])=[O:9])([O-:3])=[O:2].S(=O)(=O)(O)O>C(O)C>[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([O:15][CH2:13][CH2:6][CH2:7][CH3:8])=[O:14])[C:7](=[CH:11][CH:12]=1)[C:8]([O:10][CH2:5][CH2:4][CH2:12][CH3:11])=[O:9])([O-:3])=[O:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 691211,2-Benzenedicarboxylic acid, 4-nitro-

생성물 1

HCID 22457397HCID 22457397, 화합물수율 136.7%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
120 °C

실험 절차

4-nitrophthalic acid (2.0 g, 9.5 mmol) was dissolved in 30 ml of absolute ethanol and then 0.3 ml of concentrated sulfuric acid was added. The mixture was heated at 120° C. for 24 hours, and the solvent was evaporated under reduced pressure. The oily residue was dissolved in diethyl ether and washed three times with water and once with 10% Na2CO3 solution. The ether solution was dried over anhydrous sodium sulfate. After evaporation of the solvent, a light yellow crude solid was obtained. The crude product was purified by silica gel column chromatography (n-hexane: acetic acid =10:1) to give 2.1 g (68.4%) of di-n-butyl 4-nitrophthalate (compound 403).

후처리

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe oily residue was dissolved in diethyl ether
  3. washwashed three times with water
  4. dry with materialThe ether solution was dried over anhydrous sodium sulfate
  5. customAfter evaporation of the solvent
  6. customa light yellow crude solid was obtained
  7. customThe crude product was purified by silica gel column chromatography (n-hexane: acetic acid =10:1)

출처 및 근거

ORD 기록
ord-128edfc196634d60801854f711646ac2
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06399318B1

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