N-Methylhydrazinecarbothioamide → N-Methyl-N-[3-[3-(methylamino)-1,2,4-triazolo[4,3-b]-pyridazin-6-yl]phenyl]propanamide

HRID 35653

反応式

HRID 35653 の反応式
[CH3:1][N:2]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]2[N:14]=[N:15][C:16](Cl)=[CH:17][CH:18]=2)[CH:8]=1)[C:3](=[O:6])[CH2:4][CH3:5].[CH3:20][NH:21][C:22](=S)[NH:23][NH2:24]>C(O)C>[CH3:1][N:2]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]2[CH:18]=[CH:17][C:16]3[N:15]([C:22]([NH:21][CH3:20])=[N:23][N:24]=3)[N:14]=2)[CH:8]=1)[C:3](=[O:6])[CH2:4][CH3:5]

参加物

4

反応物 2

HCID 2723853N-MethylhydrazinecarbothioamideHCID 14280298N-methyl-N-[3-(6-chloro-3-pyridazinyl)phenyl]propanamide

生成物 1

HCID 15595694N-Methyl-N-[3-[3-(methylamino)-1,2,4-triazolo[4,3-b]-pyridazin-6-yl]phenyl]propanamide収率 16%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5.0 g of N-methyl-N-[3-(6-chloro-3-pyridazinyl)phenyl]propanamide and 3.8 g 4-methylthiosemicarbazide in 200 ml ethanol was refluxed for 18 hours. The mixture was then treated and the product chromatographed as described in Example 70. Recrystalization of the product from dichloromethane-hexane afforded 0.9 g yellow powder, mp 212°-213° C.

後処理

  1. additionThe mixture was then treated
  2. customthe product chromatographed
  3. customRecrystalization of the product from dichloromethane-hexane

出典と根拠

ORDレコード
ord-689457526f1141bbb582c037084d05f4
出典データセット
uspto-grants-1988_08
特許番号
US04767765

関連ノート

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