Ethanol hydrochloride → 1-Acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

HRID 1531972ノート

反応式

HRID 1531972 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][C:17]([OH:19])=[O:18])[CH2:5]1)(=[O:3])[CH3:2].Cl.[CH3:21][CH2:22]O>CCO>[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][C:17]([O:19][CH2:21][CH3:22])=[O:18])[CH2:5]1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 21887872Ethanol hydrochlorideHCID 222473451-Acetyl-3-(2-carboxyethyl)-4,6-dimethylindoline

生成物 1

HCID 222473291-Acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-Acetyl-3-(2-carboxyethyl)-4,6-dimethylindoline (3.4 g) was dissolved in EtOH (50 ml) and 10N HCl-EtOH (3.9 ml) was added, which was followed by refluxing for 30 min. EtOH was evaporated under reduced pressure and AcOEt (100 ml) was added. After washing with water, the mixture was dried over anhydrous sodium sulfate. AcOEt was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3/MeOH=50/1−10/1) to give 3.3 g of 1-acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline.

後処理

  1. temperatureby refluxing for 30 min
  2. customEtOH was evaporated under reduced pressure and AcOEt (100 ml)
  3. additionwas added
  4. washAfter washing with water
  5. dry with materialthe mixture was dried over anhydrous sodium sulfate
  6. customAcOEt was evaporated under reduced pressure
  7. 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-d98a421356e34045b8d0b47f7011db50
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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