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
反応条件
- 温度
- 50 °C
実験手順
To a diethyl ether solution of isopropyl magnesium bromide, chloropentafluorobenzene was added at 0 to 40° C. under nitrogen with stirring in a period of thirty minutes, such that the isopropyl magnesium bromide was in 1.03 to 1.05 molar excess of the chloropentafluorobenzene. The mixture was stirred at 47 to 53° C.; after 5 to 10 hours, bromopentafluorobenzene was added to react with the excess isopropyl magnesium bromide, and the mixture was stirred at 25° C. for 1 hour. Any excess bromo-pentafluorobenzene was back-titrated in situ with isopropyl magnesium bromide to form more C6F5MgBr. The yield of C6F5MgBr was 96.1%, and 3.9% C6F5Cl 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 was stirred at 25° C. for 1 hour
出典と根拠
- ORDレコード
- ord-ad2cee0a57154d0da73629e6118be4f6
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06248265B1
関連ノート
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