1-Bromooctane → 3-Octoxymethyl-3-methyloxetane

HRID 34965

反応式

HRID 34965 の反応式
[OH:1][CH2:2][C:3]1([CH3:7])[CH2:6][O:5][CH2:4]1.[Na].Br[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]>O1CCOCC1>[CH2:10]([O:1][CH2:2][C:3]1([CH3:7])[CH2:6][O:5][CH2:4]1)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

参加物

5

反応物 3

HCID 81401-BromooctaneHCID 1378373-Methyl-3-oxetanemethanolHCID 5360545Sodium2 回

生成物 1

HCID 144346343-Octoxymethyl-3-methyloxetane収率 58%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Into a 5 liter, three-neck flask, fitted with a stirrer, reflux condenser, and nitrogen inlet tube, were placed 245 g (2.4 mole) of 3-hydroxymethyl-3-methyloxetane and 3000 ml of p-dioxane. To this solution 47 g (2 mole) of solid sodium metal was added, and the pot temperature was raised to reflux. Heat was maintained until all of the sodium had dissolved. 400 g (2 mole) of 1-bromooctane was added, and the reflux was resumed for 3 days. The mixture was cooled to room temperature, and the solid sodium bromide was filtered off using celite. The solvent was removed by evaporation and the product was distilled at 80° C. and 0.3-mm pressure. Redistillation from calcium hydride gave 231 g of polymerizable monomer, representing a 58 percent yield.

後処理

  1. customInto a 5 liter, three-neck flask, fitted with a stirrer
  2. temperaturereflux condenser, and nitrogen inlet tube
  3. temperaturethe pot temperature was raised
  4. temperatureto reflux
  5. temperatureHeat
  6. dissolutionhad dissolved
  7. filtrationthe solid sodium bromide was filtered off
  8. customThe solvent was removed by evaporation
  9. distillationthe product was distilled at 80° C.
  10. distillationRedistillation from calcium hydride

出典と根拠

ORDレコード
ord-101502ab77eb40c4a13d0614e6644675
出典データセット
uspto-grants-1988_08
特許番号
US04764586

関連ノート

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