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Phosphorus oxychloride → 4,6-Dichloro-3-nitroquinoline

HRID 476153
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HRID 476153 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[CH:7][C:6]([N+:12]([O-:14])=[O:13])=[C:5]2O.O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:5]1[C:4]2[C:9](=[CH:10][CH:11]=[C:2]([Cl:1])[CH:3]=2)[N:8]=[CH:7][C:6]=1[N+:12]([O-:14])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178526764HCID 178526764, 화합물2회

생성물 1

HCID 106816704,6-Dichloro-3-nitroquinoline

실험 절차

6-Chloro-3-nitroquinolin-4-ol (Compound of step 2, 5 g, 22.42 mmol) in POCl3 (150 mL, 493 mmol) was stirred for 45 min at 120° C. The mixture was cooled to RT and poured slowly into ice-water. The precipitate was filtered, washed with ice-cold water, and dissolved in CH2Cl2. The organic phase was washed with cold brine and dried over Na2SO4. The organic solvent was evaporated to dryness to obtain the title compound.

후처리

  1. filtrationThe precipitate was filtered
  2. washwashed with ice-cold water
  3. dissolutiondissolved in CH2Cl2
  4. washThe organic phase was washed with cold brine
  5. dry with materialdried over Na2SO4
  6. customThe organic solvent was evaporated to dryness

출처 및 근거

ORD 기록
ord-8e3351cd1f964ade91403170bb04b6e9
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637670B2

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