Sodium Carbonate → Benzene, 1,1'-[(2-bromoethoxy)methylene]bis[4-fluoro-

HRID 1032338노트

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HRID 1032338 반응식
Br[CH:2]([C:10]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][CH:4]=1.C(=O)([O-])[O-].[Na+].[Na+].[Br:23][CH2:24][CH2:25][OH:26]>O>[F:9][C:6]1[CH:7]=[CH:8][C:3]([CH:2]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)[O:26][CH2:25][CH2:24][Br:23])=[CH:4][CH:5]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 108982-BromoethanolHCID 676651,1'-(Bromomethylene)bis(4-fluorobenzene)

생성물 1

HCID 10568186Benzene, 1,1'-[(2-bromoethoxy)methylene]bis[4-fluoro-수율 73.2%

시약·촉매·용매 1

HCID 962Water용매

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온도
130 °C

실험 절차

A mixture of 49.5 g (0.175 mole) of bromo bis(4-fluoro phenyl)methane, 22.4 g (0.21 mole) of sodium carbonate and 26.9 g (0.21 mole) of 2-bromoethanol was stirred at 130° C. for 15 hours. After cooling, the reaction mixture was taken up with water and extracted with ether. The ethereal phase was washed, dried on sodium sulfate and then concentrated dry. Distillation of the residue yielded 41.9 g (yield: 69.4%) of 1-[bis(4-fluorophenyl) methoxy]-2-bromoethane.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ether
  3. washThe ethereal phase was washed
  4. customdried on sodium sulfate
  5. concentrationconcentrated
  6. customdry
  7. distillationDistillation of the residue

출처 및 근거

ORD 기록
ord-cf0e627371b74d7bb7c0c58302ca1d8b
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04957927

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