Sodium Bicarbonate → HCID 22238274, 화합물

HRID 1743196노트

반응식

HRID 1743196 반응식
C[O:2][C:3]1[CH:8]=[C:7]([O:9]C)[CH:6]=[CH:5][C:4]=1[C:11]([C:16]1[CH:21]=[CH:20][C:19]([CH:22]([CH3:24])[CH3:23])=[CH:18][CH:17]=1)(O)[CH:12]([CH3:14])[CH3:13].C(=O)([O-])O.[Na+]>Br>[CH:22]([C:19]1[CH:18]=[CH:17][C:16]([CH:11]2[C:4]3[CH:5]=[CH:6][C:7]([OH:9])=[CH:8][C:3]=3[O:2][C:12]2([CH3:14])[CH3:13])=[CH:21][CH:20]=1)([CH3:24])[CH3:23]

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 222382771-(2,4-Dimethoxyphenyl)-1-(4-isopropylphenyl)-2-methylpropan-1-ol

생성물 1

HCID 22238274HCID 22238274, 화합물수율 51%

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

A mixture of 1-(2,4-dimethoxyphenyl)-1-(4-isopropylphenyl)-2-methylpropan-1-ol (5.58 g, 17.0 mmol) and 48% hydrobromic acid (30 mL) was heated under reflux for 24 hours in an argon atmosphere. After the reaction mixture was cooled, an aqueous saturated sodium hydrogencarbonate was added to the mixture, which was then extracted twice with ethyl acetate. The organic layers were combined, washed with brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (hexane/ethyl acetate=20/1 to 10/1) to obtain the title compound (2.43 g, yield 51%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hours in an argon atmosphere
  3. temperatureAfter the reaction mixture was cooled
  4. extractionwas then extracted twice with ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-42786e5755e34482a04c4d939650be16
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07008950B1

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