o-CRESYL GLYCIDYL ETHER → 1-(2-Methylphenoxy)-3-[1,1-dimethyl-3-(chloro-6-pyridazinyloxy)propylamino]-2-propanol

HRID 745506

반응식

HRID 745506 반응식
[NH2:1][C:2]([CH3:14])([CH3:13])[CH2:3][CH2:4][O:5][C:6]1[N:7]=[N:8][C:9]([Cl:12])=[CH:10][CH:11]=1.[CH3:15][C:16]1[CH:26]=[CH:25][CH:24]=[CH:23][C:17]=1[O:18][CH2:19][CH:20]1[O:22][CH2:21]1>CO>[CH3:15][C:16]1[CH:26]=[CH:25][CH:24]=[CH:23][C:17]=1[O:18][CH2:19][CH:20]([OH:22])[CH2:21][NH:1][C:2]([CH3:14])([CH3:13])[CH2:3][CH2:4][O:5][C:6]1[N:7]=[N:8][C:9]([Cl:12])=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 16640o-CRESYL GLYCIDYL ETHERHCID 100362353-(3-Amino-3-methylbutoxy)-6-chloropyridazine

생성물 1

HCID 103623581-(2-Methylphenoxy)-3-[1,1-dimethyl-3-(chloro-6-pyridazinyloxy)propylamino]-2-propanol수율 82.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 645 mg of 3-(3-amino-3-methylbutoxy)-6-chloropyridazine, 650 mg of 1-(2-methylphenoxy)-2,3-epoxypropane and 15 ml of methanol was refluxed for 5 hours, and the solvent was evaporated under reduced pressure. A solution of the residue in benzene was extracted with 1N hydrochloric acid. The aqueous layer was extracted with chloroform, and the organic layer was washed with 5% sodium carbonate, and dried over anhydrous sodium sulfate. The solvent was evaporated to give 938 mg of 1-(2-methylphenoxy)-3-[1,1-dimethyl-3-(chloro-6-pyridazinyloxy)propylamino]-2-propanol as an oil.

후처리

  1. temperaturewas refluxed for 5 hours
  2. customthe solvent was evaporated under reduced pressure
  3. extractionA solution of the residue in benzene was extracted with 1N hydrochloric acid
  4. extractionThe aqueous layer was extracted with chloroform
  5. washthe organic layer was washed with 5% sodium carbonate
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-e53fe69f9f624a768ba47b67fbbb6b00
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599333

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