Water → HCID 19980944, 화합물

HRID 2174161노트

반응식

HRID 2174161 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([F:10])[C:3]=1[OH:11].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].O>CCC(C)=O.CCCC[N+](CCCC)(CCCC)CCCC.[Br-]>[CH2:19]([O:11][C:3]1[C:2]([F:1])=[C:7]([F:8])[CH:6]=[C:5]([F:9])[C:4]=1[F:10])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]

참가 물질

7

반응물 4

HCID 962WaterHCID 81731-BromodecaneHCID 11430Potassium CarbonateHCID 698582,3,5,6-Tetrafluorophenol

생성물 1

HCID 19980944HCID 19980944, 화합물수율 99.6%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 6569Methyl Ethyl Ketone용매2회

실험 절차

To 20.0 g of 2,3,5,6-tetrafluorophenol (1) dissolved in 100 mL of MEK there were added 18.3 g of potassium carbonate, 4.26 g of TBAB and 32.0 g of bromodecane dissolved in 50 mL of MEK, with heating under reflux for 4 hours. After cooling and addition of water, the organic layer was separated and the aqueous layer was extracted with diethyl ether. The organic layers were combined, were washed with saturated brine, and were then dried over anhydrous magnesium sulfate. The solvent was evaporated to yield 36.8 g (120 mmol) of 4-decyloxy-2,3,5,6-tetrafluorobenzene (10).

후처리

  1. temperaturewith heating
  2. temperatureunder reflux for 4 hours
  3. temperatureAfter cooling
  4. customthe organic layer was separated
  5. extractionthe aqueous layer was extracted with diethyl ether
  6. washwere washed with saturated brine
  7. dry with materialwere then dried over anhydrous magnesium sulfate
  8. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-7ef4580e7b174b66a19a3f1fbda10f61
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09059410B2

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