3-(2-Amino-2-methylpropoxy)-6-chloropyridazine → 1-(2-Chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol

HRID 745494ノート

反応式

HRID 745494 の反応式
[NH2:1][C:2]([CH3:13])([CH3:12])[CH2:3][O:4][C:5]1[N:6]=[N:7][C:8]([Cl:11])=[CH:9][CH:10]=1.[Cl:14][C:15]1[C:25]([CH3:26])=[CH:24][CH:23]=[CH:22][C:16]=1[O:17][CH2:18][CH:19]1[O:21][CH2:20]1>CO>[Cl:14][C:15]1[C:25]([CH3:26])=[CH:24][CH:23]=[CH:22][C:16]=1[O:17][CH2:18][CH:19]([OH:21])[CH2:20][NH:1][C:2]([CH3:13])([CH3:12])[CH2:3][O:4][C:5]1[N:6]=[N:7][C:8]([Cl:11])=[CH:9][CH:10]=1

参加物

4

反応物 2

HCID 103304683-(2-Amino-2-methylpropoxy)-6-chloropyridazineHCID 233133352-[(2-Chloro-3-methylphenoxy)methyl]oxirane

生成物 1

HCID 99783091-(2-Chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol収率 66.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 6.04 g of 3-(2-amino-2-methylpropoxy)-6-chloropyridazine obtained in Example 1, (a) and 5.95 g of 1-(2-chloro-3-methylphenoxy)-2,3-epoxypropane in 120 ml of methanol was refluxed for 3 hours. The solvent was evaporated under reduced pressure. A solution of the residue in benzene was extracted with 175 ml of 0.2N hydrochloric acid. The aqueous layer was made alkaline with potassium carbonate and extracted with chloroform. The chloroform layer was dried over sodium sulfate. The solvent was evaporated and the residue (10 g) was purified by column chromatography (50 g of Florisil; eluted with chloroform) to give 7.98 g of 1-(2-chloro-3-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinyloxy)ethylamino]-2-propanol as a colorless oil.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. extractionA solution of the residue in benzene was extracted with 175 ml of 0.2N hydrochloric acid
  3. extractionextracted with chloroform
  4. dry with materialThe chloroform layer was dried over sodium sulfate
  5. customThe solvent was evaporated
  6. customthe residue (10 g) was purified by column chromatography (50 g of Florisil; eluted with chloroform)

出典と根拠

ORDレコード
ord-d970a2615e1946218829aff55aee5dab
出典データセット
uspto-grants-1986_07
特許番号
US04599333

反応ノート

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