Phenol → 2-(2-Phenoxytetrafluoro-ethyl)-1,3-dioxolane

HRID 345617

반응식

HRID 345617 반응식
[H-].[Na+].[C:3]1([OH:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH:10]([O:12][CH2:13][CH2:14]Cl)=[O:11].[F:16][C:17]([F:21])=[C:18]([F:20])[F:19]>COCCOCCOC.O>[O:9]([C:18]([F:20])([F:19])[C:17]([F:21])([F:16])[CH:10]1[O:12][CH2:13][CH2:14][O:11]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 996PhenolHCID 8301TetrafluoroethyleneHCID 24758Sodium hydrideHCID 2467482-Chloroethyl formate

생성물 1

HCID 144014502-(2-Phenoxytetrafluoro-ethyl)-1,3-dioxolane수율 57%

시약·촉매·용매 2

HCID 962Water용매HCID 8150Diglyme용매2회

실험 절차

A suspension of 17.3 g (0.36 mol) of 50% NaH in mineral oil in 100 mL of diglyme was treated with a solution of 33.9 g (0.36 mol) of phenol in 50 mL of diglyme. The resulting mixture was stirred overnight and then charged into a 400 mL metal tube along with 38.6 g (0.36 mol) of 2-chloroethyl formate and 40 g (0.40 mol) of tetrafluoroethylene. The resulting mixture was agitated for 12 h, and then added to 1 L of cold water, thereby causing the formation of layers. The lower layer was washed with water, dried over CaSO4, and distilled to afford 54.5 g (57% yield) of 2-(2-phenoxytetrafluoro-ethyl)-1,3-dioxolane, b.p. 62°-65° at 8 Pa (0.06 mm). The IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd. for C11H10F4O3 :C, 49.63; H, 3.79l F, 28.55. Found: C, 49 90; H, 3.80; F, 28.91.

후처리

  1. stirringThe resulting mixture was agitated for 12 h
  2. washThe lower layer was washed with water
  3. dry with materialdried over CaSO4
  4. distillationdistilled

출처 및 근거

ORD 기록
ord-1ef80adf2f2241d58d016862f4c661db
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05057586

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