Phenylsilane → Bis(3,5-difluorophenyl)phosphine

HRID 52764

反応式

HRID 52764 の反応式
[F:1][C:2]1[CH:3]=[C:4]([P:9]([C:11]2[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[CH:12]=2)O)[CH:5]=[C:6]([F:8])[CH:7]=1.C1([SiH3])C=CC=CC=1>>[F:17][C:15]1[CH:16]=[C:11]([PH:9][C:4]2[CH:5]=[C:6]([F:8])[CH:7]=[C:2]([F:1])[CH:3]=2)[CH:12]=[C:13]([F:18])[CH:14]=1

参加物

3

反応物 2

HCID 12752PhenylsilaneHCID 19067351Bis(3,5-difluorophenyl)phosphinous acid

生成物 1

HCID 12175518Bis(3,5-difluorophenyl)phosphine

反応条件

温度
130 °C

実験手順

Bis(3,5-difluorophenyl)phosphinous acid (4.78 g=0.0174 mole) was placed in a 50 mL round bottom flask equipped with a magnetic stirring bar and a condenser with a nitrogen inlet tube. To this was added phenylsilane (1.54 g=0.014 mole). With stirring, the reaction was heated to 130° C. for three hours. As the temperature rose, the mixture became homogeneous and remained as such. After three hours, the reaction mixture was distilled, collecting the fraction boiling at 128°-138° C. at 0.05 mm Hg. The yield of bis(3,5-difluorophenyl)phosphine was 2.45 g (54%). The 3P absorption is at -37 ppm (relative to external H3PO4).

後処理

  1. customequipped with a magnetic stirring bar and a condenser with a nitrogen inlet tube
  2. distillationthe reaction mixture was distilled
  3. customcollecting the fraction boiling at 128°-138° C. at 0.05 mm Hg
  4. customThe 3P absorption

出典と根拠

ORDレコード
ord-9ac7604dd504448ab1c4b995fe56965d
出典データセット
uspto-grants-1997_04
特許番号
US05616785

関連ノート

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