4,5-Dichloro-3-hydroxypyridazine → N-[3-(o-chlorophenoxy)-2-hydroxypropyl]-N'-[4-chloro-3-oxopyridaz-5-yl]-ethylenediamine hydrochloride

HRID 371381

反応式

HRID 371381 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[O:4][CH2:5][CH:6]([OH:12])[CH2:7][NH:8][CH2:9][CH2:10][NH2:11].[Cl:17][C:18]1[C:19](=[O:25])[NH:20][N:21]=[CH:22][C:23]=1Cl>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[O:4][CH2:5][CH:6]([OH:12])[CH2:7][NH:8][CH2:9][CH2:10][NH:11][C:23]1[CH:22]=[N:21][NH:20][C:19](=[O:25])[C:18]=1[Cl:17]

参加物

4

反応物 2

HCID 732474,5-Dichloro-3-hydroxypyridazineHCID 155809971-[(2-Aminoethyl)amino]-3-(2-chlorophenoxy)propan-2-OL

生成物 1

HCID 15580998N-[3-(o-chlorophenoxy)-2-hydroxypropyl]-N'-[4-chloro-3-oxopyridaz-5-yl]-ethylenediamine hydrochloride収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

4.9 g of N-[3-(o-chlorophenoxy)-2-hydroxy-propyl]-ethylenediamine ##STR15## are dissolved in 50 ml of ethanol. A solution of 3.3 g of 4,5-dichloropyridazin-3-one ##STR16## in 50 ml of ethanol is added to the above solution, and the mixture is then heated under reflux for 12 hours. The mixture is then concentrated in vacuo, the residue is digested with a little ethyl acetate and decanted off from the ethyl acetate, and the residue is finally recrystallised from ethanol. The N-[3-(o-chlorophenoxy)-2-hydroxypropyl]-N'-[4-chloro-3-oxopyridaz-5-yl]-ethylenediamine hydrochloride ##STR17## is thus obtained.

後処理

  1. temperaturethe mixture is then heated
  2. temperatureunder reflux for 12 hours
  3. concentrationThe mixture is then concentrated in vacuo
  4. customdecanted off from the ethyl acetate
  5. customthe residue is finally recrystallised from ethanol

出典と根拠

ORDレコード
ord-a15f75c8df9f41408cae84706636688f
出典データセット
uspto-grants-1985_07
特許番号
US04532239

関連ノート

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