反応 #58050

反応方程式

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

溶媒

dichloro-1,2-ethane

反応条件

後処理

1. 1
   その他to return to ambient temperature
2. 2
   抽出extracted with CH2Cl2
3. 3
   洗浄The organic phase is washed with saturated aqueous NaCl solution
4. 4
   乾燥dried over MgSO4
5. 5
   その他The expected product is purified by chromatography on a silica column (CH2Cl2/heptane 75/25)

実験手順

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).

出典