Water → N-Methyl-3-(benzyloxy)-benzeneethanamine

HRID 1271244ノート

反応式

HRID 1271244 の反応式
[H-].[Li+].[Al+3].[H-].[H-].[H-].[CH2:7]([O:14][C:15]1[CH:16]=[C:17]([CH2:21][CH2:22][NH:23][CH:24]=O)[CH:18]=[CH:19][CH:20]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[OH-].[Na+]>O1CCCC1>[CH2:7]([O:14][C:15]1[CH:16]=[C:17]([CH2:21][CH2:22][NH:23][CH3:24])[CH:18]=[CH:19][CH:20]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 229319731-[3-(Benzyloxy)phenyl]-2-(formylamino)ethane

生成物 1

HCID 22931944N-Methyl-3-(benzyloxy)-benzeneethanamine収率 76.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1.07 g of aluminum lithium hydride was suspended in 20 ml of tetrahydrofuran and a solution of 4.78 g of 1-[3-(benzyloxy)phenyl]-2-(formylamino)ethane in 10 ml of tetrahydrofuran was added dropwise at room temperature. The mixture was stirred at room temperature for 30 minutes and then heated at reflux for 2 hours. The reaction solution was ice-cooled and 1 ml of water, 1 ml of an aqueous 15% sodium hydroxide solution and 3 ml of water were added dropwise in order, followed by stirring for 30 minutes. The insoluble solid was removed by filtration and the solvent in the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 3.46 g of the desired compound as a pale yellow oily substance.

後処理

  1. temperatureheated
  2. temperatureat reflux for 2 hours
  3. temperaturecooled
  4. stirringby stirring for 30 minutes
  5. customThe insoluble solid was removed by filtration
  6. customthe solvent in the filtrate was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-ecf2e94bc1aa4d62bba534fd60397f3c
出典データセット
uspto-grants-2007_04
特許番号
US07205302B2

反応ノート

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