HCID 21429131, 화합물 → 5-(Trifluoromethyl)-1-benzofuran

HRID 1403444노트

반응식

HRID 1403444 반응식
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

참가 물질

3

반응물 1

HCID 21429131HCID 21429131, 화합물

생성물 1

HCID 230580725-(Trifluoromethyl)-1-benzofuran수율 93.4%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

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

출처 및 근거

ORD 기록
ord-331556b1f664427c8f7048c63039d050
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08912188B2

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