Sulfamide → N-{4-[4-(4-Pyridyl)piperazin-1-yl]phenyl}sulphamide

HRID 2232402

反応式

HRID 2232402 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[S:20](N)([NH2:23])(=[O:22])=[O:21]>O1CCOCC1>[N:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:12][CH2:13][N:8]([C:5]3[CH:4]=[CH:3][C:2]([NH:1][S:20]([NH2:23])(=[O:22])=[O:21])=[CH:7][CH:6]=3)[CH2:9][CH2:10]2)=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 82267SulfamideHCID 108904611-(4-Aminophenyl)-4-(4-pyridyl)piperazine

生成物 1

HCID 21283526N-{4-[4-(4-Pyridyl)piperazin-1-yl]phenyl}sulphamide収率 16.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of 1-(4-aminophenyl)-4-(4-pyridyl)piperazine (0.50 g) and sulphamide (1.90 g) in dioxan (30 ml) was heated under reflux for 1 hour and then evaporated. The residue was triturated with water and the mixture was filtered. The solid was crystallised from a mixture of N,N-dimethylformamide and water to give the title compound (0.11 g), m.p. 216°-219° C. Found: C,54.03; H,5.59; N,20.68. C15H19N5O2S requires: C,54.05; H,5.75; N,21.01%.

後処理

  1. temperatureunder reflux for 1 hour
  2. customevaporated
  3. customThe residue was triturated with water
  4. filtrationthe mixture was filtered
  5. customThe solid was crystallised from a mixture of N,N-dimethylformamide and water

出典と根拠

ORDレコード
ord-905b23856fc4437c8aa104a3afb1dc44
出典データセット
uspto-grants-1988_11
特許番号
US04788196

関連ノート

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