Hydroquinone → 4-(3,5-Dichloro-pyridin-2-yloxy)-phenol

HRID 249197노트

반응식

HRID 249197 반응식
Cl[C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][N:3]=1.[C:10]1([CH:17]=[CH:16][C:14]([OH:15])=[CH:13][CH:12]=1)[OH:11]>CS(C)=O.O.C1OCCOCCOCCOCCOCCOC1>[Cl:8][C:7]1[C:2]([O:11][C:10]2[CH:17]=[CH:16][C:14]([OH:15])=[CH:13][CH:12]=2)=[N:3][CH:4]=[C:5]([Cl:9])[CH:6]=1

참가 물질

6

반응물 2

HCID 785HydroquinoneHCID 27666Pyridine, 2,3,5-trichloro-

생성물 1

HCID 6208804-(3,5-Dichloro-pyridin-2-yloxy)-phenol수율 48.5%

시약·촉매·용매 3

HCID 2855718-Crown-6촉매HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

2,3,5-Trichloropyridine (69.32 g, 0.38 mol) and 18-crown-6 (4.0 g, 0.015 mol) are added to a mixture of the dipotassium salt of hydroquinone (prepared from hydroquinone (44.0 g, 0.4 mol) and potassium hydroxide (45.0 g, 0.8 mol)) in dimethyl sulfoxide (700 mL). The reaction mixture is stirred overnight at room temperature, heated at 60° C. for 21/2 hours, diluted with water and extracted with ether. The combined organic extracts are washed with water, treated with charcoal, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain the title product as a white solid (47.23 g, mp 122°-123.5° C.)

후처리

  1. temperatureheated at 60° C. for 21/2 hours
  2. extractionextracted with ether
  3. washThe combined organic extracts are washed with water
  4. additiontreated with charcoal
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b83ad9e263e941e281837bdecdd8640c
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05213606

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