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

Water → 4-Bromo-2-fluoro-5-methoxyaniline

HRID 619888
노트
인쇄 미리보기

반응식

HRID 619888 반응식
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([N+:10]([O-])=O)=[C:4]([F:13])[CH:3]=1.O.C(OCC)C>C(O)(=O)C.[Fe]>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([NH2:10])=[C:4]([F:13])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 3283Diethyl EtherHCID 132814332-Bromo-4-fluoro-5-nitroanisole

생성물 1

HCID 133631374-Bromo-2-fluoro-5-methoxyaniline수율 89%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

실험 절차

To a stirred solution of 30.0 g (0.12 mole) of 4-bromo-2-fluoro-5-methoxynitrobenzene in 200 mL of acetic acid was added 40 mL of water, followed by the portionwise addition of 30.0 g (0.54 mole) of iron filings during a 2.5 hour period. Upon complete addition, the reaction mixture was stirred at 25°-35° C. for one hour. Diethyl ether, 200 mL, was added, and the reaction mixture was filtered through a pad of diatomaceous earth. The filtrate was washed with 200 mL of water. The organic layer was separated and neutralized with solid sodium bicarbonate. The mixture was dried with magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give a residual solid. The solid was recrystallized from petroleum ether to give 23.5 g of 4-bromo-2-fluoro-5-methoxyaniline; m.p. 60°-62° C.

후처리

  1. additionUpon complete addition
  2. filtrationthe reaction mixture was filtered through a pad of diatomaceous earth
  3. washThe filtrate was washed with 200 mL of water
  4. customThe organic layer was separated
  5. dry with materialThe mixture was dried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customto give a residual solid
  9. customThe solid was recrystallized from petroleum ether

출처 및 근거

ORD 기록
ord-b8c8a65775c340c5a0c90065b97d6c4b
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04818276

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트