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Phosphorus oxychloride → HCID 178469510, 화합물

HRID 401220
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인쇄 미리보기

반응식

HRID 401220 반응식
C(O[C:4](=[O:19])[C:5](=[CH:11][NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])C.P(Cl)(Cl)(Cl)=O>>[CH2:9]([O:8][C:6]([C:5]1[CH:11]=[N:12][C:13]2[C:14]([C:4]=1[OH:19])=[CH:15][CH:16]=[CH:17][CH:18]=2)=[O:7])[CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 2643272-Phenylaminomethylene-malonic acid diethyl ester

생성물 1

HCID 178469510HCID 178469510, 화합물

반응 조건

온도
70 °C

실험 절차

A 1 L three-necked flask fitted with a mechanical stirrer was charged with 2-phenylaminomethylene-malonic acid diethyl ester (26.3 g, 0.1 mol), polyphosphoric acid (270 g) and phosphoryl chloride (750 g). The mixture was heated to about 70° C. and stirred for 4 h. The mixture was cooled to room temperature, and filtered. The residue was treated with aqueous Na2CO3 solution, filtered, washed with water and dried. 4-Hydroxyquinoline-3-carboxylic acid ethyl ester was obtained as a pale brown solid (15.2 g, 70%). The crude product was used in next step without further purification.

후처리

  1. custom
A 1 L three-necked flask fitted with a mechanical stirrer
  • temperatureThe mixture was cooled to room temperature
  • filtrationfiltered
  • additionThe residue was treated with aqueous Na2CO3 solution
  • filtrationfiltered
  • washwashed with water
  • customdried
  • 출처 및 근거

    ORD 기록
    ord-3f5ee0203f67417387c06f6b21ed0479
    출처 데이터셋
    uspto-grants-2014_06
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08741925B2

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