Isobutylene oxide → HCID 60880493, 화합물

HRID 452643노트

반응식

HRID 452643 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[H-].[Na+].[CH3:11][C:12]1([O:15][CH2:14]1)[CH3:13]>O1CCCC1.C(OCC)(=O)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:11][C:12]([CH3:14])([OH:15])[CH3:13])=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 11208Isobutylene oxideHCID 24758Sodium hydrideHCID 660494-Bromothiophenol

생성물 1

HCID 60880493HCID 60880493, 화합물수율 89%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-bromothiophenol (9.45 g, 50.0 mmol) in tetrahydrofuran (150 mL) was added sodium hydride (60% in oil, 2.20 g, 55.0 mmol) at 0° C. by small portions, and the resulting mixture was stirred for 1 hr. To this reaction mixture was added isobutylene oxide (4.91 mL, 55.0 mmol), and the resulting mixture was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=1/1) to give the title compound (11.6 g, yield 89%) as a colorless oil.

후처리

  1. stirringthe resulting mixture was stirred overnight at room temperature
  2. washwashed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by basic silica gel column chromatography (hexane/ethyl acetate=1/1)

출처 및 근거

ORD 기록
ord-85f65893c2b94321a0f3681f2d9664f8
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492378B2

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