Phosphorus oxychloride → 2-Chloro-5-(4-chlorophenyl)pyridine

HRID 1733572

반응식

HRID 1733572 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11](=O)[NH:12][CH:13]=2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:11]1[CH:10]=[CH:9][C:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)=[CH:13][N:12]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 102623725-(4-Chlorophenyl)-2-hydroxypyridine

생성물 1

HCID 100365542-Chloro-5-(4-chlorophenyl)pyridine

실험 절차

A mixture of 22.27 g. of 5-(4-chlorophenyl)-2(1H)-pyridinone and 100 ml. of phosphorus oxychloride is refluxed for 16 hours, chilled and poured onto cracked ice. The solid formed is collected by filtration and then is dissolved in chloroform. The chloroform solution is washed with water and with saturated sodium bicarbonate and then is dried over magnesium sulfate. The solvent is evaporated at reduced pressure to yield 21.1 g. of the product of the Example as a gray solid, m.p. 113°-115° C.

후처리

  1. additionA mixture of 22.27 g
  2. temperaturechilled
  3. additionpoured
  4. customThe solid formed
  5. filtrationis collected by filtration
  6. dissolutionis dissolved in chloroform
  7. washThe chloroform solution is washed with water and with saturated sodium bicarbonate
  8. dry with materialis dried over magnesium sulfate
  9. customThe solvent is evaporated at reduced pressure
  10. customto yield 21.1 g

출처 및 근거

ORD 기록
ord-664a29ce737d4a28899c2c1be96663e1
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04242515

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