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

HRID 1188646
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HRID 1188646 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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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-30694991718e479887b90637828112d6
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673948B2

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