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

HRID 1403335ノート

反応式

HRID 1403335 の反応式
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

参加物

3

反応物 1

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

生成物 1

HCID 117883225-Fluoro-1-benzofuran

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ec434952c99247b18ee9114564f94fa5
出典データセット
uspto-grants-2014_12
特許番号
US08912188B2

反応ノート

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