反応 #444901

反応方程式

indene

X-100

bromine

→

trans-2-bromoindan-1-ol

溶媒

water

反応条件

後処理

1. 1
   workup.ADDITIONmixed
2. 2
   workup.ADDITIONMixing
3. 3
   workup.ADDITIONwas added dropwise over approximately 3 hours
4. 4
   workup.STIRRINGAfter this, stirring at 60° C.
5. 5
   抽出The reaction mixture was extracted with ethyl acetate
6. 6
   workup.ADDITIONdirectly after dropwise addition of bromine
7. 7
   workup.ADDITIONafter mixing for a further 1 hour

実験手順

43.5 g of indene (92 wt %; 0.345 mol), 0.7 g of Triton X-100 and 100 ml of water were put into a 500-ml 3-mouthed flask, and mixed by stirring. Mixing was continued at 60° C. as 27.5 g of bromine (0.172 mol, 0.5 mol/mol of indene) was added dropwise over approximately 3 hours. After this, stirring at 60° C. was continued. The reaction mixture was extracted with ethyl acetate directly after dropwise addition of bromine, and after mixing for a further 1 hour. Yields of trans-2-bromoindan-1-ol were calculated from the hydrogen bromide concentrations in the aqueous phase (by gravimetric titration using silver nitrate), and the quantity of indene in the extraction layer was found by GC by means of a calibration line and used to calculate percent conversion.

出典