HCID 21429131、化合物 → 5-(Trifluoromethyl)-1-benzofuran

HRID 1403444ノート

反応式

HRID 1403444 の反応式
C(O[CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([F:16])([F:15])[F:14])=[CH:9][CH:8]=1)C>C1C=CC=CC=1>[F:14][C:13]([F:16])([F:15])[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 21429131HCID 21429131、化合物

生成物 1

HCID 230580725-(Trifluoromethyl)-1-benzofuran収率 93.4%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a mixture of benzene (100 mL) containing polyphosphoric acid (19.45 g, 57.54 mmol) was added 1-(2,2-diethoxyethoxy)-4-(trifluoromethyl)benzene (8.0 g, 28.75 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 silica gel column chromatography eluting with 1% ethyl acetate in petroleum ether to afford 5-(trifluoromethyl)-1-benzofuran (5.0 g, crude) as colorless oil.

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 silica gel column chromatography
  7. washeluting with 1% ethyl acetate in petroleum ether

出典と根拠

ORDレコード
ord-331556b1f664427c8f7048c63039d050
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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