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

HRID 76786

反応式

HRID 76786 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4427781082e3430b827ae41f560b31e3
出典データセット
uspto-grants-2014_09
特許番号
US08835639B2

関連ノート

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