Toluene → Pentafluorobenzyltriphenylphosphonium bromide

HRID 464124

反応式

HRID 464124 の反応式
C1([P:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)C=CC=CC=1.[F:20][C:21]1[C:26](C[Br:28])=[C:25]([F:29])[C:24]([F:30])=[C:23]([F:31])[C:22]=1[F:32].[C:33]1([CH3:39])[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>>[Br-:28].[F:29][C:25]1[C:26]([P+:7]([CH2:39][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)=[C:21]([F:20])[C:22]([F:32])=[C:23]([F:31])[C:24]=1[F:30]

参加物

4

反応物 3

HCID 1140TolueneHCID 11776TriphenylphosphineHCID 74484Pentafluorobenzyl bromide

生成物 1

HCID 87730649Pentafluorobenzyltriphenylphosphonium bromide収率 90%

実験手順

A five-liter, three-necked flask equipped with a mechanical stirrer, reflux condenser, and thermometer was charged with toluene (3.3 liters), triphenylphosphine (686 g, 2.62 mole), and pentafluorobenzyl bromide (343 g, 1.31 mole). The contents were stirred and heated slowly to reflux. A white precipitate formed as the reaction progressed. At the completion of the reaction the flask was cooled to ambient temperature and the solid product was filtered and washed with hot toluene (2.6 liters). These solids were dried in a vacuum desiccator to give a 90% yield of pentafluorobenzyltriphenylphosphonium bromide.

後処理

  1. customA five-liter, three-necked flask equipped with a mechanical stirrer
  2. temperaturereflux condenser
  3. temperatureheated slowly
  4. temperatureto reflux
  5. customA white precipitate formed as the reaction
  6. customAt the completion of the reaction the flask
  7. filtrationthe solid product was filtered
  8. washwashed with hot toluene (2.6 liters)
  9. customThese solids were dried in a vacuum desiccator

出典と根拠

ORDレコード
ord-1e46d549e2f34f48b3a86a51324c3fb5
出典データセット
uspto-grants-1985_10
特許番号
US04546184

関連ノート

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