1-Bromooctane → 3-Octoxymethyl-3-methyloxetane

HRID 34965

반응식

HRID 34965 반응식
[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]

참가 물질

5

반응물 3

HCID 81401-BromooctaneHCID 1378373-Methyl-3-oxetanemethanolHCID 5360545Sodium2회

생성물 1

HCID 144346343-Octoxymethyl-3-methyloxetane수율 58%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-101502ab77eb40c4a13d0614e6644675
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764586

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