2,5-Hexanedione → N-(2,5-Dimethylpyrrol-1-yl)-6-(4-methylpiperazin-1-yl)pyridazin-3-amine

HRID 1390003ノート

反応式

HRID 1390003 の反応式
[NH:1]([C:3]1[N:4]=[N:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)=[CH:7][CH:8]=1)[NH2:2].[CH3:16][C:17](=O)[CH2:18][CH2:19][C:20](=O)[CH3:21]>C(O)(=O)C>[CH3:21][C:20]1[N:2]([NH:1][C:3]2[N:4]=[N:5][C:6]([N:9]3[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]3)=[CH:7][CH:8]=2)[C:17]([CH3:16])=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 80352,5-HexanedioneHCID 13016467Pyridazine, 3-hydrazinyl-6-(4-methyl-1-piperazinyl)-

生成物 1

HCID 23275680N-(2,5-Dimethylpyrrol-1-yl)-6-(4-methylpiperazin-1-yl)pyridazin-3-amine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
70 °C

実験手順

A mixture of 7 g (35 m moles) of 3-hydrazino-6-(4-methyl-1-piperazinyl)-pyridazine and 4.1 g (36 m moles) of 2,5-hexanedione in 100 ml of acetic acid is heated for 3 hours at 70° C. The solvent is evaporated off under vacuum and the oily residue is dissolved in water and made alkaline with 10% sodium hydroxyde. The mixture is extracted with ethyl acetate and the organic layer is evaporated to dryness in vacuo. The solid residue is crystallized first from ethyl ether and then from ethyl acetate yielding 2.6 g (26%) of the product of the title which melts at 181°-182° C.

後処理

  1. customThe solvent is evaporated off under vacuum
  2. dissolutionthe oily residue is dissolved in water
  3. extractionThe mixture is extracted with ethyl acetate
  4. customthe organic layer is evaporated to dryness in vacuo
  5. customThe solid residue is crystallized first from ethyl ether

出典と根拠

ORDレコード
ord-1ed09182a629421385e573f67784e038
出典データセット
uspto-grants-1981_01
特許番号
US04247551

反応ノート

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