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

HRID 129360

반응식

HRID 129360 반응식
[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

참가 물질

4

반응물 2

HCID 74014-Methoxybenzenesulfonyl chlorideHCID 8916Decylamine

생성물 1

HCID 52013694-methoxy-n-Decylsulfamoylbenzene수율 66.9%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-35cc5ce59e954d9bae0a3b8762b75909
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05468587

연결된 노트

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