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

HRID 1032338

反応式

HRID 1032338 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cf0e627371b74d7bb7c0c58302ca1d8b
出典データセット
uspto-grants-1990_09
特許番号
US04957927

関連ノート

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