Reacción #58050

Ecuación de reacción

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

Disolventes

dichloro-1,2-ethane

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroto return to ambient temperature
2. 2
   Extracciónextracted with CH2Cl2
3. 3
   LavadoThe organic phase is washed with saturated aqueous NaCl solution
4. 4
   Secadodried over MgSO4
5. 5
   OtroThe expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)

Procedimiento

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).

Fuente