Acetic Acid → 2,4,6-Triethylbenzyl bromide

HRID 1890230노트

반응식

HRID 1890230 반응식
[CH2:1]([C:3]1[CH:8]=[C:7]([CH2:9][CH3:10])[CH:6]=[C:5]([CH2:11][CH3:12])[CH:4]=1)[CH3:2].C=O.[BrH:15].O.[C:17](O)(=O)C>C1(C)C=CC=CC=1>[CH2:11]([C:5]1[CH:6]=[C:7]([CH2:9][CH3:10])[CH:8]=[C:3]([CH2:1][CH3:2])[C:4]=1[CH2:17][Br:15])[CH3:12]

참가 물질

7

반응물 5

HCID 176Acetic Acid2회HCID 260Hydrogen BromideHCID 712FormaldehydeHCID 962WaterHCID 76021,3,5-Triethylbenzene

생성물 1

HCID 667076562,4,6-Triethylbenzyl bromide수율 84%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
45 °C

실험 절차

To a mixture of 3.00 g of 1,3,5-triethylbenzene (purity: 93%) and 5.58 g of acetic acid, 0.82 g of paraformaldehyde and 4.7 mL of a 33% solution of hydrogen bromide in acetic acid were added. This mixture was heated at 45° C. for 7.5 hours under stirring. After the reaction mixture was cooled to room temperature, 16.8 g of water and 16.8 g of toluene were added thereto. The reaction mixture was separated. The organic layer was washed sequentially with 11.2 g of water, a mixture of 5.6 g of an aqueous saturated sodium hydrogen carbonate solution and 5.6 g of water, and 11.2 g of water, dried over anhydrous magnesium sulfate, and then concentrated to obtain 4.72 g of 2,4,6-triethylbenzyl bromide (GC-area: 84%) as a yellow oil.

후처리

  1. additionwere added
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. customThe reaction mixture was separated
  4. washThe organic layer was washed sequentially with 11.2 g of water
  5. additiona mixture of 5.6 g of an aqueous saturated sodium hydrogen carbonate solution and 5.6 g of water, and 11.2 g of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-dce1f1f1881a41c7a16c0d619a96225d
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507410B2

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