Sulfuric Acid → 5-[Bis-(4-Chlorophenyl)-Methyl]-2-Pyridone

HRID 1390333

반응식

HRID 1390333 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](O)[C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[OH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1.S(=O)(=O)(O)O.C(OCC)(=O)C>O>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=2)[C:21]2[CH:22]=[CH:23][C:18](=[O:17])[NH:19][CH:20]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 70334,4'-DichlorobenzhydrolHCID 8857Ethyl AcetateHCID 178516071HCID 178516071, 화합물

생성물 1

HCID 227487685-[Bis-(4-Chlorophenyl)-Methyl]-2-Pyridone

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
200 °C

실험 절차

Combine 50.6 g. (0.2 mole) of 4,4'-dichlorobenzhydrol with 57.1 g. (0.6 mole) of 2-hydroxy pyridine, with stirring heat to 200° C. and add dropwise 1.0 ml. of concentrated sulfuric acid. Increase the reaction temperature to 240°-250° C. and maintain at that temperature range while collecting water emanating from the reaction. Cool the reaction mixture, add a mixture of ethyl acetate and water with stirring and separate the liquid phases. Dry the organic phase, reduce the volume of ethyl acetate, cool to precipitate the crude product, yield 43 g. Crystallization from ethanol affords the product of this step, m.p. 211°-215° C.

후처리

  1. additionadd dropwise 1.0 ml
  2. temperatureIncrease the reaction temperature to 240°-250° C.
  3. temperaturemaintain at that temperature range
  4. customwhile collecting water emanating
  5. customfrom the reaction
  6. temperatureCool the reaction mixture
  7. additionadd
  8. customseparate the liquid phases
  9. customDry the organic phase
  10. temperaturecool
  11. customto precipitate the crude product, yield 43 g
  12. customCrystallization from ethanol
  13. customaffords the product of this step, m.p. 211°-215° C.

출처 및 근거

ORD 기록
ord-b4ec73929dc04ea69628776727c52530
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04138488

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