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Bromine → 1-Bromo-2,3,4,5-tetramethoxy-6-methylbenzene

HRID 2268437
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HRID 2268437 반응식
[Br:1]Br.[CH3:3][O:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([O:12][CH3:13])=[C:7]([O:14][CH3:15])[C:6]=1[O:16][CH3:17]>C(O)(=O)C>[Br:1][C:10]1[C:9]([CH3:11])=[C:8]([O:12][CH3:13])[C:7]([O:14][CH3:15])=[C:6]([O:16][CH3:17])[C:5]=1[O:4][CH3:3]
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참가 물질

4

반응물 2

HCID 24408BromineHCID 98777642,3,4,5-Tetramethoxytoluene

생성물 1

HCID 125607691-Bromo-2,3,4,5-tetramethoxy-6-methylbenzene수율 83.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bromine (46.7 g, 0.292 mols) was dropwise added to a solution of 1,2,3,4-tetramethoxy-5-methylbenzene (51.6 g, 0.243 mols) in acetic acid (100 ml) at room temperature, and the reaction mixture was stirred for 15 minutes and then concentrated in vacuo. The residue was diluted with ethyl acetate, and the organic layer was washed with water, a saturated aqueous sodium bicarbonate solution, water and a saturated aqueous sodium chloride solution, then dried, and concentrated in vacuo. The thus-obtained crude product was purified by silica gel column chromatography (hexane:ethyl acetate=20:1) to obtain the entitled compound (59.1 g) as an oil.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue was diluted with ethyl acetate
  3. washthe organic layer was washed with water
  4. dry with materiala saturated aqueous sodium bicarbonate solution, water and a saturated aqueous sodium chloride solution, then dried
  5. concentrationconcentrated in vacuo
  6. customThe thus-obtained crude product
  7. customwas purified by silica gel column chromatography (hexane:ethyl acetate=20:1)

출처 및 근거

ORD 기록
ord-06dce7c814e64274b58dc462733d890d
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06326369B1

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