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

HRID 1966816ノート

反応式

HRID 1966816 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ce7d606590aa4187ac24494bc354bece
出典データセット
uspto-grants-2013_04
特許番号
US08420666B2

反応ノート

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