Sodium Hydroxide → 1-Acetyl-3-(2-hydroxyethyl)-4,6-dimethylindoline

HRID 1531968ノート

反応式

HRID 1531968 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[C:10]([CH3:13])[CH:11]=2)[CH:6]([CH2:15][CH2:16][O:17]C(=O)C)[CH2:5]1)(=[O:3])[CH3:2].[OH-].[Na+]>C(Cl)(Cl)Cl.CO.O>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[C:10]([CH3:13])[CH:11]=2)[CH:6]([CH2:15][CH2:16][OH:17])[CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 222473471-Acetyl-3-(2-acetoxyethyl)-4,6-dimethylindoline

生成物 1

HCID 222473161-Acetyl-3-(2-hydroxyethyl)-4,6-dimethylindoline収率 70.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21584188Chloroform methanol溶媒

実験手順

1-Acetyl-3-(2-acetoxyethyl)-4,6-dimethylindoline (2.0 g) was dissolved in a mixture of CHCl3/MeOH=1/1 (25 ml), and a solution of NaOH (1.5 g) in water (5 ml) was added, which was followed by stirring at room temperature for 1 hr. The solvent was evaporated under reduced pressure. CHCl3 (100 ml) was added, and the mixture was washed with water and dried over anhydrous sodium sulfate. CHCl3 was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3/MeOH=50/1−10/1) to give 1.2 g of 1-acetyl-3-(2-hydroxyethyl)-4,6-dimethylindoline.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. additionCHCl3 (100 ml) was added
  3. washthe mixture was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customCHCl3 was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluent: CHCl3/MeOH=50/1−10/1)

出典と根拠

ORDレコード
ord-9ff24629f6804f9d904842dec1160db5
出典データセット
uspto-grants-2001_03
特許番号
US06200988B1

反応ノート

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