4-Chloro-3-nitrobenzenesulfonamide → 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide

HRID 1035870

反応式

HRID 1035870 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].Cl.Cl.[CH3:17][N:18]1[CH2:23][CH2:22][N:21]([NH2:24])[CH2:20][CH2:19]1.CN(C)CCN(C)C>O1CCOCC1>[CH3:17][N:18]1[CH2:23][CH2:22][N:21]([NH:24][C:2]2[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][C:3]=2[N+:12]([O-:14])=[O:13])[CH2:20][CH2:19]1

参加物

5

反応物 3

HCID 73244-Chloro-3-nitrobenzenesulfonamideHCID 8037N,N,N',N'-TetramethylethylenediamineHCID 1982214-Methylpiperazin-1-ylamine dihydrochloride hydrate

生成物 1

HCID 47377414-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A 50 mL round-bottomed flask was charged with 4-chloro-3-nitrobenzenesulfonamide (1 g, 4.23 mmol), 4-methylpiperazin-1-amine dihydrochloride (1 g, 5.32 mmol), and N1,N1,N2,N2-tetramethylethane-1,2-diamine (3 mL, 20.01 mmol) in dioxane (10 mL). The reaction mixture was refluxed for 12 hours. After this time, the reaction mixture was cooled to room temperature, the salt filtered off via a Buchner funnel, and the solvent removed in vacuo. The crude product was added to a silica gel column (Analogix, SF65-200 g) and purified by eluting with 0-5% methanol in dichloromethane.

後処理

  1. temperatureThe reaction mixture was refluxed for 12 hours
  2. filtrationthe salt filtered off via a Buchner funnel
  3. customthe solvent removed in vacuo
  4. additionThe crude product was added to a silica gel column (Analogix
  5. customSF65-200 g) and purified
  6. washby eluting with 0-5% methanol in dichloromethane

出典と根拠

ORDレコード
ord-17071ac8d1b14bcea7eb326a207c1607
出典データセット
uspto-grants-2013_10
特許番号
US08546399B2

関連ノート

読み込み中…