Triethanolamine → 1-Ethenyl-4-nitrobenzene

HRID 1589339

반응식

HRID 1589339 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([CH2:8][CH2:9]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].N(CCO)(CCO)CCO>O>[N+:1]([C:4]1[CH:12]=[CH:11][C:7]([CH:8]=[CH2:9])=[CH:6][CH:5]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 7618TriethanolamineHCID 792664-Nitrophenethyl bromide

생성물 1

HCID 74811-Ethenyl-4-nitrobenzene수율 89.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 500 ml 3-neck round bottom flask was fitted with a thermometer and steam distillation apparatus. The flask was charged with 12.5 g (0.054 mol) of 4-nitrophenethyl bromide, 75 ml (0.565 mol) of triethanolamine and 50 ml of water. The reaction mixture was heated to reflux and the mixture was allowed to slowly steam distill. Approximately 100 mg of hydroquinone was added to the distillate collected in order to prevent polymerization. The distillate was extracted three times with diethyl ether and the combined organic phases were washed with water, 1N hydrochloric acid, water, and a saturated sodium chloride solution in sequence. The organic phase was dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure to provide 7.193 g of 4-nitrostyrene as an oil which solidified upon cooling. Additional quantities of this material were prepared by the general procedure above.

후처리

  1. customA 500 ml 3-neck round bottom flask was fitted with a thermometer and steam distillation apparatus
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux
  4. distillationdistill
  5. additionApproximately 100 mg of hydroquinone was added to the distillate
  6. customcollected in order
  7. custompolymerization
  8. extractionThe distillate was extracted three times with diethyl ether
  9. washthe combined organic phases were washed with water, 1N hydrochloric acid, water
  10. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  11. customevaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-e6458f9d347e4d8bb0a16098a58b2c27
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04569801

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