Iodine → HCID 178418276、化合物

HRID 1750

反応式

HRID 1750 の反応式
[Mg:1].II.[Br:4]CCBr.Br[C:9]1[CH:14]=CC(OC)=[CH:11][CH:10]=1.[CH2:17]1[CH2:21][O:20][CH2:19][CH2:18]1>>[CH2:11]([Mg:1][Br:4])[C:10]1[CH:18]=[CH:17][C:21]([O:20][CH3:19])=[CH:14][CH:9]=1

参加物

6

反応物 5

HCID 807IodineHCID 77304-BromoanisoleHCID 78391,2-DibromoethaneHCID 8028TetrahydrofuranHCID 5462224Magnesium

生成物 1

HCID 178418276HCID 178418276、化合物

反応条件

温度
20 °C

実験手順

Magnesium (36 g, 1.5 mol), iodine (a few crystals) and THF (1 L) were heated under nitrogen, with stirring, at reflux for 15 min. The mixture was cooled to 20° C., stirring stopped, and 1,2-dibromoethane (2.5 ml) added. After an exothermic reaction was observed (a few min) stirring was restarted which was accompanied by a rise in temperature to 35° C. The mixture was cooled to 20° C. and 4-bromoanisole slowly added over 1 h at 14°-18° C. with cooling. Stirring was continued for 10 min after the addition was complete.

後処理

  1. temperatureat reflux for 15 min
  2. stirringstirring
  3. customAfter an exothermic reaction
  4. stirringstirring
  5. customwas accompanied by a rise in temperature to 35° C
  6. temperatureThe mixture was cooled to 20° C.
  7. temperaturewith cooling
  8. stirringStirring
  9. additionafter the addition

出典と根拠

ORDレコード
ord-f12406699295447fa245b2a1d83d7703
出典データセット
uspto-grants-1998_03
特許番号
US05726315

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