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Phosphorus tribromide → HCID 57429660, 화합물

HRID 889022
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HRID 889022 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH:9]2[CH2:11][CH:10]2[CH2:12]O)[CH:6]=[CH:7][CH:8]=1.[Br:16]P(Br)Br>C(OCC)C>[Br:16][CH2:12][CH:10]1[CH2:11][CH:9]1[C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:15])([F:14])[F:1])[CH:4]=1
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참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 53275778HCID 53275778, 화합물

생성물 1

HCID 57429660HCID 57429660, 화합물수율 145.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

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온도
0 °C

실험 절차

[2-(3-Trifluoromethyl-phenyl)-cyclopropyl]-methanol obtained in step 1 (0.250 g, 1.15 mmol) was taken in diethyl ether (4 ml) and cooled to 0° C. Tribromo phosphine (0.06 ml, 0.64 mmol) in diethyl ether (4 ml) was added slowly at 0° C. and stirred at 15-20° C. for 2 hrs. Reaction mixture was quenched with saturated NaHCO3 solution (20 ml) and extracted with diethyl ether. Organic layer was washed with saturated brine solution, dried over Na2SO4, and evaporated under vacuum to get 1-(2-bromomethyl-cyclopropyl)-3-trifluoromethyl-benzene (0.26 g, 80%) as a sticky mass.

후처리

  1. customReaction mixture
  2. customwas quenched with saturated NaHCO3 solution (20 ml)
  3. extractionextracted with diethyl ether
  4. washOrganic layer was washed with saturated brine solution
  5. dry with materialdried over Na2SO4
  6. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-2bb57fc029c84df882d974ec945325de
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08252797B2

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