Water → 2-Isopropyl-3-methoxyphenol

HRID 1677308ノート

反応式

HRID 1677308 の反応式
O[C:2]([C:5]1[C:10]([O:11][CH3:12])=[CH:9][CH:8]=[CH:7][C:6]=1[OH:13])([CH3:4])[CH3:3].O.C([O-])=O.[NH4+]>C(O)(=O)C.[Pd]>[CH:2]([C:5]1[C:10]([O:11][CH3:12])=[CH:9][CH:8]=[CH:7][C:6]=1[OH:13])([CH3:4])[CH3:3]

参加物

6

反応物 3

HCID 962WaterHCID 2723923Ammonium formateHCID 595986452-(1-Hydroxy-1-methyl-ethyl)-3-methoxy-phenol

生成物 1

HCID 144655792-Isopropyl-3-methoxyphenol収率 92%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

To a solution of 2-(1-Hydroxy-1-methyl-ethyl)-3-methoxy-phenol dissolved in acetic acid (50 mL) was added 10% palladium on charcoal (500 mg), water (6 mL), and ammonium formate (7.82 g, 124 mmol). After refluxing for 1 hour, the reaction was cooled and filtered through celite. The celite pad was washed with ethyl acetate (500 mL). Water (300 mL) was added to the filtrate, and the mixture was basified (pH=8) using solid sodium bicarbonate. The ethyl acetate layer was collected and washed with water, brine, dried using anhydrous sodium sulfate and concentrated to yield 2-Isopropyl-3-methoxy-phenol (3.68 g, 92%) as pale yellow solid.

後処理

  1. temperatureAfter refluxing for 1 hour
  2. temperaturethe reaction was cooled
  3. filtrationfiltered through celite
  4. washThe celite pad was washed with ethyl acetate (500 mL)
  5. additionWater (300 mL) was added to the filtrate
  6. customThe ethyl acetate layer was collected
  7. washwashed with water, brine
  8. customdried
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-cbde5c8d743a4ccfbe365dc3446ed345
出典データセット
uspto-grants-2011_08
特許番号
US08008313B2

反応ノート

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