تفاعل #1435753
ord-0b42858fd1174b349b6ad7db8808e9e5
معادلة التفاعل
3-(6,7-dimethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-propylamine dihydrochloride
N,N-diisopropylethylamine
3-Chloro-4,6-difluorobenzenesulfonyl chloride
→
solid
المردود 87.0%
5-Chloro-N-[3-(6,7-dimethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-propyl]-2,4-difluoro-benzenesulfonamide
المردود 87.0%
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1غسيلThe resulting solution was washed with water (3×20 mL)
- 2تجفيفdried over Na2SO4
- 3أخرىevaporated to dryness
- 4workup.DISSOLUTIONThe free base was dissolved in 2-propanol (5 mL)
- 5أخرىThe product was crystallized in 2-propanol (5 mL)
- 6ترشيحcollected by filtration, and vacuum
- 7أخرىdried
الإجراء التجريبي
A solution of 3-(6,7-dimethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-propylamine dihydrochloride (323 mg, 1 mmol), N,N-diisopropylethylamine (517 mg, 4 mmol) in CH2Cl2(15 mL), was added 3-Chloro-4,6-difluorobenzenesulfonyl chloride (259 mg, 1.05 mmol) and was stirred overnight at room temperature. The resulting solution was washed with water (3×20 mL) and dried over Na2SO4, and evaporated to dryness. The free base was dissolved in 2-propanol (5 mL). The product was crystallized in 2-propanol (5 mL) collected by filtration, and vacuum dried to give a white solid (401 mg, 87%).