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Water → 1-(Bromomethyl)-2-phenoxybenzene

HRID 397819
ノート
印刷プレビュー

反応式

HRID 397819 の反応式
P(Br)(Br)[Br:2].[O:5]([C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH2:14]O)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.O>O1CCOCC1>[O:5]([C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH2:14][Br:2])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
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 962WaterHCID 24614Phosphorus tribromide2 回HCID 36601112-Phenoxybenzyl alcohol

生成物 1

HCID 226754691-(Bromomethyl)-2-phenoxybenzene収率 89.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

Phosphorus tribromide (5.5 ml, 57.1 mmol) was added dropwise over a period of 10 min to a solution of 2-phenoxybenzylalcohol (4.08 g, 20.4 mmol) in dioxane (165 ml). The reaction mixture was stirred for 40 min. Another portion of phosphorus tribromide (5.5 ml, 57.1 mmol) was added. The reaction mixture was stirred for 56 hours at room temperature. It was cooled to 0° C. Water (45 ml) was added carefully. The reaction mixture was stirred for 30 min at room temperature. The mixture was extracted with ethyl acetate (100 ml). The ethyl acetate phase was washed with 1 N hydrochloric acid. The combined aqueous layers were extracted with ethyl acetate. The combined organic layers were washed with a saturated aqueous soludtion of sodium hydrogen carbonate (100 ml) and dried over magnesium sulphate. The solvent was removed in vacuo. The crude product was purified by flash chromatography on silica (90 g), using ethyl acetate/heptane (1:3) as eluent, to give 4.80 g of 2-phenoxybenzyl bromide.

後処理

  1. stirringThe reaction mixture was stirred for 56 hours at room temperature
  2. stirringThe reaction mixture was stirred for 30 min at room temperature
  3. extractionThe mixture was extracted with ethyl acetate (100 ml)
  4. washThe ethyl acetate phase was washed with 1 N hydrochloric acid
  5. extractionThe combined aqueous layers were extracted with ethyl acetate
  6. washThe combined organic layers were washed with a saturated aqueous soludtion of sodium hydrogen carbonate (100 ml)
  7. dry with materialdried over magnesium sulphate
  8. customThe solvent was removed in vacuo
  9. customThe crude product was purified by flash chromatography on silica (90 g)

出典と根拠

ORDレコード
ord-b99a3554ad02456299eadecc3616c018
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06610721B2

反応ノート

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