1-Naphthol → HCID 19819480, 화합물

HRID 1031051

반응식

HRID 1031051 반응식
[F:1][C:2]1[C:7]([C:8]2[C:13]([F:14])=[C:12]([F:15])[C:11](F)=[C:10]([F:17])[C:9]=2[F:18])=[C:6]([F:19])[C:5]([F:20])=[C:4](F)[C:3]=1[F:22].[C:23]1([OH:33])[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:26]=[CH:25][CH:24]=1.[C:34](=[O:37])([O-])[O-].[K+].[K+]>CC(N(C)C)=O>[C:23]1([O:33][C:4]2[C:5]([F:20])=[C:6]([F:19])[C:7]([C:8]3[C:9]([F:18])=[C:10]([F:17])[C:11]([O:37][C:34]4[C:2]5[C:7](=[CH:6][CH:5]=[CH:4][CH:3]=5)[CH:8]=[CH:9][CH:10]=4)=[C:12]([F:15])[C:13]=3[F:14])=[C:2]([F:1])[C:3]=2[F:22])[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:26]=[CH:25][CH:24]=1

참가 물질

5

반응물 3

HCID 70051-NaphtholHCID 11430Potassium CarbonateHCID 67949Decafluorobiphenyl

생성물 1

HCID 19819480HCID 19819480, 화합물수율 78.8%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
140 °C

실험 절차

The monomer 4,4'-bis(1-naphthoxy)octafluorobiphenyl (8FNE) was prepared by the following procedure. A 100 mL round bottom flask was charged with decafluorobiphenyl (3.01 g, 0.0090 mole), 1-naphthol (2.60 g, 0.0181 mole), potassium carbonate (2.95 g, 0.0218 mole), and DMAc (40 g). The mixture was heated with stirring at about 140° C. for 2 hr and then cooled to room temperature, filtered, and poured into toluene (100 mL). The toluene solution was washed with 5% sodium hydroxide (50 mL) and then twice with deionized water (2×100 mL). After drying with magnesium sulfate and filtering, it was concentrated by rotary evaporation to yield a red solid. The solid was recrystallized from DMAc/water, filtered, and dried to yield 8FNE (3.9 g, 78.8% yield; m.p. 189°-191 ° C.; GC/MS m+ /e 582).

후처리

  1. temperatureThe mixture was heated
  2. temperaturecooled to room temperature
  3. filtrationfiltered
  4. additionpoured into toluene (100 mL)
  5. washThe toluene solution was washed with 5% sodium hydroxide (50 mL)
  6. dry with materialAfter drying with magnesium sulfate
  7. filtrationfiltering
  8. concentrationit was concentrated by rotary evaporation
  9. customto yield a red solid
  10. customThe solid was recrystallized from DMAc/water
  11. filtrationfiltered
  12. customdried
  13. customto yield 8FNE (3.9 g, 78.8% yield; m.p. 189°-191 ° C.; GC/MS m+ /e 582)

출처 및 근거

ORD 기록
ord-b83995380f6a455f8884199078f4019d
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05108840

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