3,6-Dichloropyridazine → 1-(2-Methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinylamino)ethylamino]-2-propanol

HRID 745509ノート

反応式

HRID 745509 の反応式
[CH3:1][C:2]1[CH:18]=[CH:17][CH:16]=[CH:15][C:3]=1[O:4][CH2:5][CH:6]([OH:14])[CH2:7][NH:8][C:9]([CH3:13])([CH3:12])[CH2:10][NH2:11].[Cl:19][C:20]1[N:21]=[N:22][C:23](Cl)=[CH:24][CH:25]=1>C1C=CC=CC=1>[CH3:1][C:2]1[CH:18]=[CH:17][CH:16]=[CH:15][C:3]=1[O:4][CH2:5][CH:6]([OH:14])[CH2:7][NH:8][C:9]([CH3:13])([CH3:12])[CH2:10][NH:11][C:23]1[N:22]=[N:21][C:20]([Cl:19])=[CH:25][CH:24]=1

参加物

4

反応物 2

HCID 673313,6-DichloropyridazineHCID 100607882-Propanol, 1-[(2-amino-1,1-dimethylethyl)amino]-3-(2-methylphenoxy)-

生成物 1

HCID 100217191-(2-Methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinylamino)ethylamino]-2-propanol収率 67.8%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
110 °C

実験手順

To 1.58 g of 1-(2-methylphenoxy)-3-(1,1-dimethyl-2-aminoethylamino)-2-propanol heated at 110° C. in an oil bath with stirring was added 934 mg of 3,6-dichloropyridazine little by little. After heating at 110° C. for 1 hour, the reaction mixture was dissolved in benzene, and extracted with 1N hydrochloric acid. The aqueous layer was made alkaline with potassium carbonate, and extracted with chloroform. The chloroform layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated to give 1.55 g of 1-(2-methylphenoxy)-3-[1,1-dimethyl-2-(3-chloro-6-pyridazinylamino)ethylamino]-2-propanol as an oil.

後処理

  1. extractionextracted with 1N hydrochloric acid
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-10f16b323fc24e5990ae31f32d0b0969
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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