تفاعل #331706

ord-b8fd1201b5654d798122c4747976812a

معادلة التفاعل

CS(=O)(=O)Cl
Methanesulphonyl chloride
CN(C)c1cccc(N)c1
N,N-dimethyl-1,3-phenylenediamine
[Na+].[OH-]
sodium hydroxide
CN(C)c1cccc(NS(C)(=O)=O)c1
material
المردود 79.0%
CN(C)c1cccc(NS(C)(=O)=O)c1
N-[3-(dimethylamino)phenyl]methanesulphonamide
المردود 79.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe mixture was extracted with chloroform (3×15 cm3)
  2. 2
    تجفيفThe combined extracts were dried over sodium sulphate
  3. 3
    ترشيحfiltered
  4. 4
    أخرىthe solvent removed under reduced pressure

الإجراء التجريبي

Methanesulphonyl chloride (838 mg, 7.35 mmol) was added slowly to a cooled solution (5° C.) of N,N-dimethyl-1,3-phenylenediamine (1.00 g, 7.35 mmol) and sodium hydroxide (5M, 1.5 cm3) in water (10 cm3). The reaction was allowed to warm to room temperature overnight. The mixture was extracted with chloroform (3×15 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:20 methanol/dichloromethane) gave the target material as a brown oil (1.24 g, 79%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08658665B2uspto-grants-2014_02