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Carbon Tetrachloride → 3-(Chloromethyl)-5-[3,5-bis(trifluoromethyl)phenyl]isoxazole

HRID 2102152
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HRID 2102152 반응식
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:4]=[C:5]([C:13]2[O:17][N:16]=[C:15]([CH2:18]O)[CH:14]=2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:42]>>[Cl:42][CH2:18][C:15]1[CH:14]=[C:13]([C:5]2[CH:4]=[C:3]([C:2]([F:21])([F:20])[F:1])[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=2)[O:17][N:16]=1
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참가 물질

4

반응물 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 57800356{5-[3,5-bis(Trifluoromethyl)phenyl]-3-isoxazolyl}methanol

생성물 1

HCID 578002023-(Chloromethyl)-5-[3,5-bis(trifluoromethyl)phenyl]isoxazole

반응 조건

온도
75 °C

실험 절차

To a solution of {5-[3,5-bis(trifluoromethyl)phenyl]-3-isoxazolyl}methanol (Example 323B) (0.100 g, 0.32 mmol) in dry carbon tetrachloride (15 mL) was added PS-triphenylphosphine (0.292 g, 2.2 mmol/g, 0.64 mmol). The reaction was heated at 75° C. overnight. The resin was filtered and washed with carbon tetrachloride. Concentration in vacuo afforded the title compound, which was used for the next step without further purification.

후처리

  1. filtrationThe resin was filtered
  2. washwashed with carbon tetrachloride
  3. concentrationConcentration in vacuo

출처 및 근거

ORD 기록
ord-17e5e8b08d6a44cb892837d19890c4cb
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07572820B2

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