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Nitric Acid → 4-(Difluoromethoxy)-2-nitrophenol

HRID 2060026
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HRID 2060026 반응식
[F:1][CH:2]([F:11])[O:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.[N+:12]([O-])([OH:14])=[O:13]>ClCCCl>[F:1][CH:2]([F:11])[O:3][C:4]1[CH:5]=[CH:6][C:7]([OH:10])=[C:8]([N+:12]([O-:14])=[O:13])[CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 27741244-(Difluoromethoxy)phenol

생성물 1

HCID 594440714-(Difluoromethoxy)-2-nitrophenol수율 85.9%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매2회

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온도
0 °C

실험 절차

4-(Difluoromethoxy)phenol (500 mg, 3.12 mmol) was dissolved in DCE (3 mL). The reaction mixture was cooled to 0° C. and nitric acid (0.488 mL, 10.92 mmol) was added dropwise over 10 min. The reaction mixture was stirred for a further hour at 0° C., then poured into an ice/water mix (5 g in 5 mL). DCE (10 mL) was added and the layers separated. The organic layer was dried (MgSO4) and evaporated to dryness to give a crude brown oil (550 mg). Material was carried forward without further purification, as no separation between products was found in TLC solvent systems used.

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후처리

  1. additionmix (5 g in 5 mL)
  2. customthe layers separated
  3. dry with materialThe organic layer was dried (MgSO4)
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-b48fad9de59947a783edb5f9a12f0c60
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08278328B2

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