反応式
C([Mg:4][Br:5])(C)C.Cl[C:7]1[C:12]([F:13])=[C:11]([F:14])[C:10]([F:15])=[C:9]([F:16])[C:8]=1[F:17].BrC1C(F)=C(F)C(F)=C(F)C=1F>C(OCC)C>[C:7]1([Mg:4][Br:5])[C:12]([F:13])=[C:11]([F:14])[C:10]([F:15])=[C:9]([F:16])[C:8]=1[F:17]参加物
実験手順
To a diethyl ether solution of isopropyl magnesium bromide, chloropentafluorobenzene is added at 0° C. to 40° C. under nitrogen with stirring in a period of thirty minutes, such that the isopropyl magnesium bromide is in 1.03 to 1.05 molar excess of the chloropentafluorobenzene. The mixture is stirred at 47° C. to 53° C.; after 5 to 10 hours, bromopentafluorobenzene is added to react with the excess isopropyl magnesium bromide, and the mixture is stirred at 25° C. for 1 hour. Any excess bromopentafluorobenzene is back-titrated in situ with isopropyl magnesium bromide to form more C6F5MgBr. The yield of C6F5MgBr is 96.1%, and 3.9% C6F5C1 remained, as determined by 19F NMR, using C6H5CF3 as a reference; no trace of iPrMgBr was seen with 1H NMR.
後処理
- stirringthe mixture is stirred at 25° C. for 1 hour
出典と根拠
- ORDレコード
- ord-59893ca8f471490d9b159cb2b5e1c4a3
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06129863
関連ノート
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