Reaktion #58050

Reaktionsgleichung

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

Lösungsmittel

dichloro-1,2-ethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto return to ambient temperature
2. 2
   Extraktionextracted with CH2Cl2
3. 3
   WaschenThe organic phase is washed with saturated aqueous NaCl solution
4. 4
   Trocknendried over MgSO4
5. 5
   SonstigeThe expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)

Vorschrift

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).

Quelle