تفاعل #58050

معادلة التفاعل

product

{3-[(5,5-Dioxido-2,3,3a,4-tetrahydro-1H-pyrrolo[2,1-c][1,2,4]-benzothiadiazin-7-yl)oxy]phenyl}methanamine hydrochloride

2,5-dimethoxytetrahydrofuran

water

AcOH

→

7-[3-(1H-Pyrrol-1-ylmethyl)phenoxy]-2,3,3a,4-tetrahydro-1H-pyrrolo[2,1-c][1,2,4]benzothiadiazine 5,5-dioxide

المذيبات

dichloro-1,2-ethane

ظروف التفاعل

المعالجة

1. 1
   أخرىto return to ambient temperature
2. 2
   استخلاصextracted with CH2Cl2
3. 3
   غسيلThe organic phase is washed with saturated aqueous NaCl solution
4. 4
   تجفيفdried over MgSO4
5. 5
   أخرىThe expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)

الإجراء التجريبي

200 mg (0.58 mmol) of the product obtained in Example 1, in the form of the free amine, and 105 μl (0.81 mmol) of 2,5-dimethoxytetrahydrofuran are added to a two-phase mixture of 2.5 ml of water, 0.95 ml of AcOH and 2.85 ml of dichloro-1,2-ethane. The mixture is stirred at 80° C. for 2 hours, allowed to return to ambient temperature and extracted with CH2Cl2. The organic phase is washed with saturated aqueous NaCl solution and dried over MgSO4. The expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25).

المصدر