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

HRID 2356654노트

반응식

HRID 2356654 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6e293970af944d609abb954eacd082e2
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07759366B2

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