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Phosphorus oxychloride → HCID 20142081, 화합물

HRID 649117
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HRID 649117 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([O:12][C:13]3[CH:24]=[CH:23][C:16]([O:17][CH:18]([CH3:22])[C:19]([NH2:21])=O)=[CH:15][CH:14]=3)[CH:8]=[N:9]2)=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)=O.C(=O)(O)[O-].[Na+]>O>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([O:12][C:13]3[CH:14]=[CH:15][C:16]([O:17][CH:18]([CH3:22])[C:19]#[N:21])=[CH:23][CH:24]=3)[CH:8]=[N:9]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 20142073HCID 20142073, 화합물

생성물 1

HCID 20142081HCID 20142081, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-[4-(7-Chloroquinolin-3-yloxy)phenoxy]propionamide (see Example 23) (1.2 g) was added slowly with stirring to phosphorus oxychloride (10 ml) at 20° C. The mixture was heated briefly to the boiling point then poured on to water and neutralized carefully with aqueous sodium bicarbonate solution. Extraction with ethyl acetate gave, after drying and evaporation, the crude product as a pale yellow oil. Purification by chromatography on silica gel gave 2-[4-(7-chloroquinolin-3-yloxy)phenoxy]propionitrile, characterised by its proton magnetic resonance spectrum (Table 3).

후처리

  1. temperatureThe mixture was heated briefly to the boiling point
  2. extractionExtraction with ethyl acetate
  3. customgave
  4. customafter drying
  5. customevaporation
  6. customPurification by chromatography on silica gel

출처 및 근거

ORD 기록
ord-ca5d741527734ef1b5c0ea44036cf7f3
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04738710

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