Thionyl Chloride → 1,1'-(Chloromethylene)bis(4-fluorobenzene)

HRID 414482

反応式

HRID 414482 の反応式
[F:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](O)[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.S(Cl)([Cl:19])=O>O>[F:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([Cl:19])[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 1230494,4'-Difluorobenzhydryl alcohol

生成物 1

HCID 27237731,1'-(Chloromethylene)bis(4-fluorobenzene)収率 90.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 5.00 g (22.7 mmol) of 4,4'-difluorobenzhydrol was added 16.5 ml (227 mmol) of thionyl chloride in the atmosphere of argon, and the mixture was stirred at room temperature for 30 minutes. To the resulting mixture was added water followed by extraction with benzene. The organic layer was successively washed with saturated sodium hydrogen carbonate solution and water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue thus obtained was subjected to column chromatography on silica gel. There was yielded 4.90 g (20.5 mmol) of 4,4'-difluorobenzhydryl chloride from the fraction eluted with benzene.

後処理

  1. extractionfollowed by extraction with benzene
  2. washThe organic layer was successively washed with saturated sodium hydrogen carbonate solution and water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue thus obtained

出典と根拠

ORDレコード
ord-3105e40af57f46429c343abecd5a1306
出典データセット
uspto-grants-1988_12
特許番号
US04792553

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