反应 #43389

反应方程式

tetrahydro-pyrrolo[1,2-a]imidazole-2,5-dione

K2CO3

Iodobenzene

Ethyl acetate

→

title compound

收率 11.7%

1-Phenyl-tetrahydro-1H-pyrrolo[1,2-a]imidazole-2,5-dione

收率 11.7%

溶剂

N-methylpyrrolidone

反应条件

后处理

1. 1
   温度The suspension was heated in a microwave apparatus (250 Watt) for 45 min
2. 2
   过滤the solid was filtered
3. 3
   洗涤The organic phase was washed with water
4. 4
   萃取the aqueous phase was re-extracted with CH2Cl2
5. 5
   干燥dried over Na2SO4
6. 6
   过滤filtered
7. 7
   浓缩concentrated to dryness
8. 8
   其他The residue was triturated with isopropyl ether
9. 9
   过滤The solid was filtered
10. 10
    其他triturated with water
11. 11
    过滤filtered

实验过程

To a solution of tetrahydro-pyrrolo[1,2-a]imidazole-2,5-dione (1 g, 7.14 mmol; prepared as described in J. Med. Chem. 36, 4214-4220, 1994,) in N-methylpyrrolidone (NMP, 12 cc), CuI (0.2 g, 1.05 mmol), K2CO3 (1 g, 7.14 mmol) and Iodobenzene (5 g, 24.5 mmol) were added under stirring. The suspension was heated in a microwave apparatus (250 Watt) for 45 min. Ethyl acetate was added to the suspension and the solid was filtered. The organic phase was washed with water and the aqueous phase was re-extracted with CH2Cl2. The organic phases were gathered and dried over Na2SO4, filtered and concentrated to dryness. The residue was triturated with isopropyl ether. The solid was filtered, triturated with water and filtered to yield 0.18 g of the title compound, mp=185-188° C.

来源