Реакция #58050

Уравнение реакции

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

Растворители

dichloro-1,2-ethane

Условия реакции

Обработка

1. 1
   Другоеto return to ambient temperature
2. 2
   Экстракцияextracted with CH2Cl2
3. 3
   ПромывкаThe organic phase is washed with saturated aqueous NaCl solution
4. 4
   Сушкаdried over MgSO4
5. 5
   ДругоеThe expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)

Методика

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).

Источник