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Phosphorus oxychloride → HCID 22643158, 화합물

HRID 2414764
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HRID 2414764 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)[CH:8]=[C:7]2O)([O-:3])=[O:2].P(Cl)(Cl)([Cl:24])=O>O>[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)[CH:8]=[C:7]2[Cl:24])([O-:3])=[O:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychloride2회HCID 178526468HCID 178526468, 화합물

생성물 1

HCID 22643158HCID 22643158, 화합물수율 84%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

6-Nitro-2-(3-fluoro-phenyl)-quinolin-4-ol, 5.2 g (16.3 mmoles), was placed in a 500 mL three-neck round-bottom flask equipped with a condenser, magnetic stirrer and nitrogen inlet. To this was added 15.2 mL (25.0 g, 163 mmoles, 10 equiv.) of phosphorus oxychloride with stirring. The mixture was heated to 110° C. for 4 hr. At the end of this time the reaction was cooled to room temperature and water was cautiously added dropwise until all of the POCl3 was consumed. The product crystallised from the water and solids were collected by filtration. The solids were washed with water, placed in a 250 mL Erlenmeyer and triturated with water. After collection by filtration, washing with water, and drying in a vacuum oven, 4.6 g (84%) of the product was obtained.

후처리

  1. customequipped with a condenser, magnetic stirrer and nitrogen inlet
  2. temperatureAt the end of this time the reaction was cooled to room temperature
  3. customwas consumed
  4. customThe product crystallised from the water and solids
  5. filtrationwere collected by filtration
  6. washThe solids were washed with water
  7. customtriturated with water
  8. customAfter collection
  9. filtrationby filtration
  10. washwashing with water
  11. customdrying in a vacuum oven

출처 및 근거

ORD 기록
ord-437d8b53cdaa4f1796c54a5e7976cb23
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06815447B2

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