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Phosphorus tribromide → 1-(Bromomethyl)-2,3,5-triiodobenzene

HRID 58355
ノート
印刷プレビュー

反応式

HRID 58355 の反応式
P(Br)(Br)[Br:2].[I:5][C:6]1[C:13]([I:14])=[CH:12][C:11]([I:15])=[CH:10][C:7]=1[CH2:8]O.O.C(Cl)Cl>O1CCCC1>[I:5][C:6]1[C:13]([I:14])=[CH:12][C:11]([I:15])=[CH:10][C:7]=1[CH2:8][Br:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24614Phosphorus tribromideHCID 34957432,3,5-Triiodobenzyl alcoholHCID 21908982Water methylene chloride

生成物 1

HCID 534030771-(Bromomethyl)-2,3,5-triiodobenzene収率 85.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

A solution of phosphorous tribromide (3.8 ml, 40 mmol) was added dropwise to a solution of 2,3,5-triiodobenzyl alcohol 1 (9.72 g, 20 mmol) in dry tetrahydrofuran (50 ml) at 0° C. under dry nitrogen gas flow. The reaction mixture was stirred 5 minutes at 0° C., then 20 minutes at room temperature (18° C.), then cold H2O/DCM (60160 ml) was added. The resulting aqueous phase was extracted with dichloromethane (2×10 ml). The combined organic extracts were washed with NaHCO3 aq (20 ml) and H2O (20 ml) then dried (Na2SO4), filtered and concentrated. The white solid was also washed with cold methanol (45 ml). 9.35 g of 2,3,5-triiodobenzyl bromide in the form of a white clean solid was obtained in 85% yield.

後処理

  1. extractionThe resulting aqueous phase was extracted with dichloromethane (2×10 ml)
  2. washThe combined organic extracts were washed with NaHCO3 aq (20 ml) and H2O (20 ml)
  3. dry with materialthen dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. washThe white solid was also washed with cold methanol (45 ml)

出典と根拠

ORDレコード
ord-4346e0a624cc4077a7a9da9db4c8f90a
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434800B2

反応ノート

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