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Boron trifluoride etherate → HCID 58869153, 화합물

HRID 2355212
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HRID 2355212 반응식
[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH:18](O)[CH2:19][Si](C)(C)C)=[C:12]([Br:25])[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.B(F)(F)F.CCOCC>C(Cl)Cl>[C:1]1([S:7]([C:10]2[CH:15]=[CH:14][C:13]([CH2:16][CH2:17][CH:18]=[CH2:19])=[C:12]([Br:25])[CH:11]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8000Boron trifluoride etherateHCID 66917402HCID 66917402, 화합물

생성물 1

HCID 58869153HCID 58869153, 화합물수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a solution of 4-(4-benzenesulfonyl-2-bromo-phenyl)-1-trimethylsilanyl-butan-2-ol (4.38 g) in DCM (80 mL) was added BF3.OEt2 (3.76 mL) at 0° C. under N2 atmosphere. The reaction was stirred at 0° C. for 1 h it was then quenched by addition of NaHCO3 (saturated solution). The mixture was extracted twice with DCM and the combined extracts were washed with water, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified via flash chromatography (hexane/EtOAc, 9/1) to afford 4-benzenesulfonyl-2-bromo-1-but-3-enyl-benzene (3.38 g, 93% yield).

후처리

  1. customwas then quenched by addition of NaHCO3 (saturated solution)
  2. extractionThe mixture was extracted twice with DCM
  3. washthe combined extracts were washed with water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified via flash chromatography (hexane/EtOAc, 9/1)

출처 및 근거

ORD 기록
ord-b15589c765b6444782507b5eb4e3f507
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754759B2

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