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Allyl iodide → Butyl 1-allylcyclopropane-1-sulfonate

HRID 73393
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HRID 73393 반응식
[CH:1]1([S:4]([O:7][CH2:8][CH2:9][CH2:10][CH3:11])(=[O:6])=[O:5])[CH2:3][CH2:2]1.[CH2:12]([Li])[CH2:13][CH2:14]C.C(I)C=C>C1COCC1>[CH2:14]([C:1]1([S:4]([O:7][CH2:8][CH2:9][CH2:10][CH3:11])(=[O:6])=[O:5])[CH2:3][CH2:2]1)[CH:13]=[CH2:12]
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참가 물질

5

반응물 3

HCID 11166Allyl iodideHCID 10464888Butyl cyclopropanesulfonateHCID 178418339Butyllithium

생성물 1

HCID 59386376Butyl 1-allylcyclopropane-1-sulfonate수율 69%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

To a solution of 1-butyl cyclopropanesulfonate (4.8 g, 24.9 mmol) in THF at −78° C. was added simultaneously butyllithium solution (15.6 ml, 24.9 mmol, 1.6M, THF) and allyl iodide (24.9 mmol) under nitrogen atmosphere. The reaction mixture was stirred 2 hours at −78° C. and 3 hours at room temperature. The volatiles were evaporated under reduced pressure and the residue extracted with CH2Cl2 (100 ml). The extract was washed with water, dried (MgSO4) and evaporated. The residue was purified over silica gel chromatography (eluants: hexane/CH2Cl2) to obtain the titled product (3.75 g, 69.0%) as a colorless oil, 1H NMR (300 MHz, CDCl3): δ 5.6 (m, 1H), 5.13-5.08 (t, 2H), 4.21 (t, 2H), 2.65 (d, 2H), 1.7 (m, 2H), 1.4 (m, 4H), 0.93 (m, 5H).

후처리

  1. customThe volatiles were evaporated under reduced pressure
  2. extractionthe residue extracted with CH2Cl2 (100 ml)
  3. washThe extract was washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue was purified over silica gel chromatography (eluants: hexane/CH2Cl2)

출처 및 근거

ORD 기록
ord-d91d8ed404e84d39b56aac3d09d5d6d1
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829052B2

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