反応 #1943458

反応方程式

ketone

3'-Acetylspiro(cyclopentane-1,1'-indene)

→

title compound

3'-(α-Bromoacetyl)spiro(cyclopentane-1,1'-indene)

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他Precipitated salts are removed by filtration
2. 2
   濃縮the filtrate is concentrated to a small volume
3. 3
   workup.ADDITIONWater (200 ml) is added
4. 4
   抽出the mixture is extracted three times with diethyl ether
5. 5
   その他After drying the solvent
6. 6
   その他is evaporated
7. 7
   その他yielding a semi-crystalline residue
8. 8
   その他Crystallization from methanol

実験手順

Pyrrolidone hydrotribromide [(pyrrolidone)3HBr3 ] is added at about 20° C. to the ketone from step (b) (12 g) in tetrahydrofuran (1500 ml) containing 10 drops of concentrated sulphuric acid. The mixture is stirred for 24 hours. Precipitated salts are removed by filtration and the filtrate is concentrated to a small volume. Water (200 ml) is added and the mixture is extracted three times with diethyl ether. After drying the solvent is evaporated, yielding a semi-crystalline residue. Crystallization from methanol gives the pure bromoacetyl title compound, m.p. 75°-77° C.

出典