反応 #2186180

ord-987832814a6d4de2a92306ae98e01851

反応方程式

Oc1cccc(Cl)c1F
compound ( b5 )
Oc1cccc(Cl)c1F
3-chloro-2-fluorophenol
[Na+].[OH-]
sodium hydroxide
CCOS(=O)(=O)OCC
diethyl sulfate
CCOc1cccc(Cl)c1F
1-chloro-3-ethoxy-2-fluorobenzene

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITover 1 hour in a temperature range of 25 to 35° C.
  2. 2
    その他The resulting organic layer was collected
  3. 3
    洗浄washed with 200 mL of water in three times
  4. 4
    その他by drying

実験手順

The compound (b5) was added dropwise to a reactor having 1,200 g of a 10% sodium hydroxide aqueous solution placed therein over 30 minutes in a temperature range of 20 to 40° C. Thereafter, 462 g of diethyl sulfate was added dropwise thereto over 1 hour in a temperature range of 25 to 35° C., followed by stirring for 5 hours in that temperature range. The resulting organic layer was collected and washed with 200 mL of water in three times, followed by drying, to obtain 505 g of 1-chloro-3-ethoxy-2-fluorobenzene (b44). The resulting liquid was colorless.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07569258B2uspto-grants-2009_08