Water → Phenol, 5-[(2-hydroxyethyl)amino]-4-methoxy-2-methyl-

HRID 1029997ノート

反応式

HRID 1029997 の反応式
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[CH:7][C:6]=1[N:13]1[CH2:17][CH2:16][O:15]C1=O.O>C(O)(=O)C>[CH3:11][C:9]1[CH:10]=[C:5]([O:4][CH3:3])[C:6]([NH:13][CH2:17][CH2:16][OH:15])=[CH:7][C:8]=1[OH:12]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 19821132HCID 19821132、化合物

生成物 1

HCID 9794190Phenol, 5-[(2-hydroxyethyl)amino]-4-methoxy-2-methyl-収率 45.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
70 °C

実験手順

10 ml of 5N sodium hydroxide was heated to 70° C., and 2.76 g (12.4 mmol) of N-(2-methoxy-4-methyl-5-hydroxyphenyl)-1,3-oxazolidin-2-one was added thereto, and then the resulting mixture was stirred at 70° C. for 1 hour. After allowing to cool, 40 ml of water was poured into the reaction mixture, and acetic acid was added thereto until no further crystals were precipitated. The crystals were filtered, washed with water and recrystallized from the solvent mixture of water/ethanol (4:1, by volume). Thus, 1.10 g (5.6 mmol) of 2-methyl-4-methoxy-5-(β-hydroxyethylamino)phenol was obtained. The yield was 45%.

後処理

  1. temperatureto cool
  2. additionwas added
  3. customuntil no further crystals were precipitated
  4. filtrationThe crystals were filtered
  5. washwashed with water
  6. customrecrystallized from the solvent mixture of water/ethanol (4:1, by volume)

出典と根拠

ORDレコード
ord-a04b393520c14199922277890d2a3cfc
出典データセット
uspto-grants-1992_04
特許番号
US05104414

反応ノート

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