반응 #58050

반응 방정식

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

용매

dichloro-1,2-ethane

반응 조건

후처리

1. 1
   기타to return to ambient temperature
2. 2
   추출extracted with CH2Cl2
3. 3
   세척The organic phase is washed with saturated aqueous NaCl solution
4. 4
   건조dried over MgSO4
5. 5
   기타The expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)

실험 절차

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).

출처