Water → HCID 19980944、化合物

HRID 2174161ノート

反応式

HRID 2174161 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 19980944HCID 19980944、化合物収率 99.6%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 6569Methyl Ethyl Ketone溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7ef4580e7b174b66a19a3f1fbda10f61
出典データセット
uspto-grants-2015_06
特許番号
US09059410B2

反応ノート

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