Sodium Carbonate → 1-Bromo-2-(bromomethyl)-3,5-dichlorobenzene

HRID 2356654ノート

反応式

HRID 2356654 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[CH2:10]O.P(Br)(Br)[Br:13].C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[CH2:10][Br:13]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 24614Phosphorus tribromideHCID 14153164(2-Bromo-4,6-dichlorophenyl)methanol

生成物 1

HCID 104260681-Bromo-2-(bromomethyl)-3,5-dichlorobenzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

3.1 g of the benzyl alcohol 35.4 were dissolved in 40 ml of dry dichloromethane and admixed dropwise at 5° C. with a solution of 0.455 ml of phosphorus tribromide in 10 ml of dichloromethane. The reaction mixture was stirred overnight and then neutralized with 5 ml of a saturated aqueous sodium carbonate solution. The organic phase was removed, dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel with n-heptane as the eluent. 2-Bromo-4,6-dichlorobenzyl bromide 35.3 was obtained.

後処理

  1. customThe organic phase was removed
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel with n-heptane as the eluent

出典と根拠

ORDレコード
ord-6e293970af944d609abb954eacd082e2
出典データセット
uspto-grants-2010_07
特許番号
US07759366B2

反応ノート

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