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

HRID 745506

反応式

HRID 745506 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e53fe69f9f624a768ba47b67fbbb6b00
出典データセット
uspto-grants-1986_07
特許番号
US04599333

関連ノート

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