홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ethyl bromoacetate → Ethyl 2-(5-fluoro-2-nitrophenoxy)acetate

HRID 247772
노트
인쇄 미리보기

반응식

HRID 247772 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([OH:8])[CH:7]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21]>C(#N)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([CH:7]=1)[O:8][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 99375-Fluoro-2-nitrophenolHCID 11430Potassium Carbonate

생성물 1

HCID 13752803Ethyl 2-(5-fluoro-2-nitrophenoxy)acetate수율 89.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a mixture consisting of 5-fluoro-2-nitrophenol (47.1 g), acetonitrile (300 ml) and potassium carbonate (46 g) was added ethyl bromoacetate (60.1 g) dropwise at a temperature from 50° to 60° C., followed by a five-hour refluxing under heating and then filtration under cooling. The resulting filtrate was subjected to distillation under reduced pressure, and then dissolved in toluene (350 ml). The resulting toluene solution was washed with water, a 5% aqueous solution of potassium hydroxide, and water, in that order, followed by drying with magnesium sulfate and the toluene was distilled off therefrom under reduced pressure. The residue was distilled under reduced pressure to collect a fraction boiling at from 154° to 156° C., so as to obtain ethyl 5-fluoro-2-nitrophenoxyacetate (65.3 g). The whole quantity of the reaction product was dissolved in ethanol (8.1 l), followed by addition thereto of a solution of ammonium chloride (60 g) and water (400 ml). To the resulting mixture was added zinc dust (60.5 g) portionwise at a temperature of from 20° to 30° C.

후처리

  1. waitfollowed by a five-hour
  2. temperaturerefluxing
  3. temperatureunder heating
  4. filtrationfiltration
  5. temperatureunder cooling
  6. distillationThe resulting filtrate was subjected to distillation under reduced pressure
  7. dissolutiondissolved in toluene (350 ml)
  8. washThe resulting toluene solution was washed with water
  9. dry with materialby drying with magnesium sulfate
  10. distillationthe toluene was distilled off
  11. distillationThe residue was distilled under reduced pressure
  12. customto collect a fraction
  13. customboiling at from 154° to 156° C.

출처 및 근거

ORD 기록
ord-dc388e3085664314a2d3ace37e34c634
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05207818

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트