Water → 2-(5-Tert-butyl-2-hydroxy-4-nitrophenyl)-2-methylpropanoic acid

HRID 76786

반응식

HRID 76786 반응식
C(=O)(OC)[O:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[C:6]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:5][C:4]=1[C:16]([CH3:21])([CH3:20])[C:17](N)=O.[OH2:25].[OH-:26].[Na+]>CO>[C:12]([C:6]1[C:7]([N+:9]([O-:11])=[O:10])=[CH:8][C:3]([OH:2])=[C:4]([C:16]([CH3:20])([CH3:17])[C:21]([OH:26])=[O:25])[CH:5]=1)([CH3:13])([CH3:14])[CH3:15]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 595441632-(1-Amino-2-methyl-1-oxopropan-2-yl)-4-tert-butyl-5-nitrophenyl methyl carbonate

생성물 1

HCID 595441502-(5-Tert-butyl-2-hydroxy-4-nitrophenyl)-2-methylpropanoic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a mixture of compound 17 (7.3 g, 21.6 mmol) in methanol (180 mL) was added water (18 mL) and NaOH (8.64 g, 216 mmol). The solution was heated and maintained at reflux for 3 days. The solvent was evaporated in vacuo and the residue was dissolved in 140 mL of water. Then the solution was acidified to pH 2 by the addition of 2N HCl. The aqueous phase was extracted with ethyl acetate (100 mL×3), and the combined organic phases were washed with water and brine, dried over anhydrous Na2SO4 and then concentrated to give compound 18 as a yellow solid, which was used in the next reaction without further purification.

후처리

  1. temperatureThe solution was heated
  2. temperaturemaintained
  3. temperatureat reflux for 3 days
  4. customThe solvent was evaporated in vacuo
  5. dissolutionthe residue was dissolved in 140 mL of water
  6. additionThen the solution was acidified to pH 2 by the addition of 2N HCl
  7. extractionThe aqueous phase was extracted with ethyl acetate (100 mL×3)
  8. washthe combined organic phases were washed with water and brine
  9. dry with materialdried over anhydrous Na2SO4
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4427781082e3430b827ae41f560b31e3
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835639B2

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