4-Methoxybenzenesulfonyl chloride → 4-methoxy-n-Decylsulfamoylbenzene

HRID 129360

反応式

HRID 129360 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9](Cl)(=[O:11])=[O:10])=[CH:5][CH:4]=1.[CH2:13]([NH2:23])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22]>N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9](=[O:11])(=[O:10])[NH:23][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 74014-Methoxybenzenesulfonyl chlorideHCID 8916Decylamine

生成物 1

HCID 52013694-methoxy-n-Decylsulfamoylbenzene収率 66.9%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Commercially available 4-methoxybenzenesulfonylchloride (Aldrich; 25 g, 0.12 moles) is added portionwise to a solution of decylamine (Kodak; 19 g, 0.12 moles) in pyridine (75 mL). The heterogeneous reaction mixture is stirred overnight at room temperature and poured into dilute HCl/ice water (1.5 L). After stirring 30 minutes, the light orange solid is isolated by filtration, washed with water and air dried. Recrystallization from ethanol (Norite) affords 26.3 g (66% yield) of the desired product as golden platelets, mp 53°-54.5° C. NMR (CDCl3) d 0.8-0.95 (t, 3H's); 1.1-1.6 (m, 16H's); 2.8-3.0 (t, 2H's); 3.9 (s, 3H's); 6.95-7.0 (d, 2H's); 7.75-7.85 (d, 2H's).

後処理

  1. stirringAfter stirring 30 minutes
  2. customthe light orange solid is isolated by filtration
  3. washwashed with water and air
  4. customdried
  5. customRecrystallization from ethanol (Norite)

出典と根拠

ORDレコード
ord-35cc5ce59e954d9bae0a3b8762b75909
出典データセット
uspto-grants-1995_11
特許番号
US05468587

関連ノート

読み込み中…