反応 #2186177

反応方程式

ethanol

potassium hydroxide

toluene

compound ( b2 )

2-chloro-1,3-difluorobenzene

→

2-chloro-1-ethoxy-3-fluorobenzene

溶媒

water

反応条件

後処理

1. 1
   その他in a temperature range of 50 to 60° C.
2. 2
   workup.WAITover 1 hour in a temperature range of 80 to 85° C.
3. 3
   workup.STIRRINGby stirring for 5 hours at 80° C
4. 4
   温度After cooling
5. 5
   その他the resulting reaction mixture to 25° C.
6. 6
   workup.ADDITIONwell mixed
7. 7
   workup.WAITthe mixture was left at rest
8. 8
   その他to separate into an organic layer
9. 9
   その他After collecting the resulting organic layer, 500 mL of toluene
10. 10
    workup.ADDITIONwas newly added to the aqueous mixture
11. 11
    workup.ADDITIONwell mixed
12. 12
    抽出to extract again the compound
13. 13
    workup.ADDITIONThe toluene solution was added to the organic layer
14. 14
    洗浄After washing the organic layer with water in three times
15. 15
    workup.DISTILLATIONthe resulting organic layer was distilled under reduced pressure

実験手順

560 g of potassium hydroxide and 23 g of tetramethylammonium chloride (TMAC) were added to a reactor having 2,000 mL of ethanol placed therein in a temperature range of 50 to 60° C., followed by stirring for 30 minutes in that temperature range. Thereafter, the solution was heated to 80° C., and 594 g of a compound (b2) was added thereto over 1 hour in a temperature range of 80 to 85° C., followed by stirring for 5 hours at 80° C. After cooling the resulting reaction mixture to 25° C., 1,000 mL of toluene and 500 mL of water were added thereto and well mixed, and the mixture was left at rest to separate into an organic layer and an aqueous layer. After collecting the resulting organic layer, 500 mL of toluene was newly added to the aqueous mixture and well mixed, and the mixture was subjected to the same operation to extract again the compound contained in the aqueous layer. The toluene solution was added to the organic layer. After washing the organic layer with water in three times, the resulting organic layer was distilled under reduced pressure to obtain 606 g of 2-chloro-1-ethoxy-3-fluorobenzene (b43). The resulting liquid was colorless and had a boiling point of 98 to 99° C./8 mmHg.

出典