1-(2,2-Diethoxyethoxy)-4-fluorobenzene → 5-Fluoro-1-benzofuran

HRID 1403335노트

반응식

HRID 1403335 반응식
C(O[CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1)C>C1C=CC=CC=1>[F:13][C:10]1[CH:9]=[CH:8][C:7]2[O:6][CH:5]=[CH:4][C:12]=2[CH:11]=1

참가 물질

3

반응물 1

HCID 114475181-(2,2-Diethoxyethoxy)-4-fluorobenzene

생성물 1

HCID 117883225-Fluoro-1-benzofuran

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a mixture of benzene (200 mL) containing polyphosphoric acid (80 g, 236.69 mmol) was added 2-(4-fluoro-phenoxy)-acetaldehyde diethyl acetal (45 g, 197.37 mmol). The mixture was stirred vigorously while being heated to reflux for 2.5 hours. The reaction mixture was cooled to room temperature and decanted from the polyphosphoric acid. The solvent was removed under vacuum to give the residue, which was purified by a silica gel column with 1% ethyl acetate in petroleum ether to afford 5-fluorobenzofuran as colorless oil (14.0 g, crude).

후처리

  1. temperaturewhile being heated
  2. temperatureto reflux for 2.5 hours
  3. customdecanted from the polyphosphoric acid
  4. customThe solvent was removed under vacuum
  5. customto give the residue, which
  6. customwas purified by a silica gel column with 1% ethyl acetate in petroleum ether

출처 및 근거

ORD 기록
ord-ec434952c99247b18ee9114564f94fa5
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08912188B2

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