Benzene → 2-Methylene-5,8-dioxaspiro[3.4]octane

HRID 1966816노트

반응식

HRID 1966816 반응식
Br[CH2:2][CH:3]1[CH2:6][C:5]2([O:10][CH2:9][CH2:8][O:7]2)[CH2:4]1.[OH-].[Na+].C1C=CC=CC=1>O>[CH2:2]=[C:3]1[CH2:6][C:5]2([O:10][CH2:9][CH2:8][O:7]2)[CH2:4]1

참가 물질

5

반응물 3

HCID 241BenzeneHCID 14798Sodium HydroxideHCID 667332822-(Bromomethyl)-5,8-dioxaspiro[3.4]octane

생성물 1

HCID 667332232-Methylene-5,8-dioxaspiro[3.4]octane

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 2-(bromomethyl)-5,8-dioxaspiro[3.4]octane (1.3 gm, 6.28 mmol) (step e), polyethylene glycol (PEG-600) (0.5 gm), 50% aqueous sodium hydroxide solution (5 ml) and benzene was refluxed for about 12 hours. The reaction mixture was cooled, diluted with water and extracted with diethyl ether. The organic layer was washed with brine, dried over sodium sulphate and concentrated under reduced pressure to get a crude product, which was purified by column chromatography.

후처리

  1. temperaturewas refluxed for about 12 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with diethyl ether
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ce7d606590aa4187ac24494bc354bece
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08420666B2

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