Bromine → 5-Bromo-3-(tert-butyl)-2-hydroxybenzaldehyde

HRID 1296019노트

반응식

HRID 1296019 반응식
[Br:1]Br.[C:3]([C:7]1[C:8]([O:15]COC)=[C:9]([CH:12]=[CH:13][CH:14]=1)[CH:10]=[O:11])([CH3:6])([CH3:5])[CH3:4]>CO>[Br:1][C:13]1[CH:14]=[C:7]([C:3]([CH3:6])([CH3:5])[CH3:4])[C:8]([OH:15])=[C:9]([CH:12]=1)[CH:10]=[O:11]

참가 물질

4

반응물 2

HCID 24408BromineHCID 22930050HCID 22930050, 화합물

생성물 1

HCID 7970065-Bromo-3-(tert-butyl)-2-hydroxybenzaldehyde수율 111%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

Bromine (747 g) was gradually added to a solution of the 3-(tert-butyl)-2-(methoxymethoxy)benzaldehyde (1247 g, 4.67 mol) in methanol (4000 ml) while cooling on ice. After stirring at 20° C. for 1 hour, the solvent was distilled off under reduced pressure, ethyl acetate was added to the residue, the mixture was washed with water, saturated sodium aqueous hydrogencarbonate and brine in that order and the organic layer was dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure to yield a crude product of the title compound (1333 g) as a red oil.

후처리

  1. temperaturewhile cooling on ice
  2. distillationthe solvent was distilled off under reduced pressure, ethyl acetate
  3. additionwas added to the residue
  4. washthe mixture was washed with water, saturated sodium aqueous hydrogencarbonate and brine in that order
  5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationThe organic layer was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3b9cde35ea9f4b3fb439de6be3084343
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07244730B2

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