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Nitric Acid → 2-Chloro-4-fluoro-5-nitrophenyl methyl carbonate

HRID 450455
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HRID 450455 반응식
[C:1](=[O:13])([O:11][CH3:12])[O:2][C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:4]=1[Cl:10].[N+:14]([O-])([OH:16])=[O:15]>OS(O)(=O)=O>[C:1](=[O:13])([O:11][CH3:12])[O:2][C:3]1[CH:8]=[C:7]([N+:14]([O-:16])=[O:15])[C:6]([F:9])=[CH:5][C:4]=1[Cl:10]
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참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 104884382-Chloro-4-fluoro-methoxycarbonyloxybenzene

생성물 1

HCID 37866902-Chloro-4-fluoro-5-nitrophenyl methyl carbonate수율 90%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

To a suspension of 2-chloro-4-fluorophenyl methyl carbonate (110 g, 0.54 mol) in conc. H2SO4 (50 mL) was slowly added a mixture comprised of cone. H2SO4 (40 mL) and fuming HNO3 (40.8 mL, 0.89 mol). The resultant mixture was stirred for 30 min at 0° C. The reaction mixture was poured into ice water and the precipitated solid was collected by filtation and washed with water to give 2-chloro-4-fluoro-5-nitrophenyl methyl carbonate (120 g, 90% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.45 (d, J=7.2 Hz, 1H), 8.12 (d, J=10.8 Hz, 1H), 3.89 (s, 3H); MS (ESI) m/z: 250.1 (MAI).

후처리

  1. additionwas slowly added a mixture
  2. customthe precipitated solid was collected by filtation
  3. washwashed with water

출처 및 근거

ORD 기록
ord-793e3faafbd849a89d8b3657e391e20a
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486951B2

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