Ammonia → {4-[2-(Diethylamino)ethoxy]phenyl}methanamine

HRID 215754

反応式

HRID 215754 の反応式
[CH2:1]([N:3]([CH2:6][CH2:7][O:8][C:9]1[CH:16]=[CH:15][C:12]([CH:13]=O)=[CH:11][CH:10]=1)[CH2:4][CH3:5])[CH3:2].[NH3:17]>C(O)C.[Ni]>[CH2:1]([N:3]([CH2:6][CH2:7][O:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][NH2:17])=[CH:11][CH:10]=1)[CH2:4][CH3:5])[CH3:2]

参加物

5

反応物 2

HCID 222AmmoniaHCID 4116744-(2-(Diethylamino)-Ethoxy)-Benzaldehyde

生成物 1

HCID 235944{4-[2-(Diethylamino)ethoxy]phenyl}methanamine収率 65%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To the solution of 4-diethylaminoethoxybenzaldehyde X in 180 ml 10% solution of ammonia in anhydrous ethanol, 4.5 g RaNi was added and the mixture was heated to 80° C. at the pressure 68 atm in the autoclave under hydrogen input to the reaction mixture under stirring for 12 hours. The mixture was cooled, the catalyst was filtered off, washed with ethanol. The solvent was distilled off from the solution and the distillation residue was purified by distillation under the reduced pressure. Afforded 13 g (65%) of 4-diethylaminoethoxybenzylamine XI. Colourless fluid 138-140° C./0.5 torr, n20D=1.520. Lit. [6.7] reports 130° C./0.3 torr, n20D=1.5220.

後処理

  1. temperatureThe mixture was cooled
  2. filtrationthe catalyst was filtered off
  3. washwashed with ethanol
  4. distillationThe solvent was distilled off from the solution
  5. distillationthe distillation residue was purified by distillation under the reduced pressure

出典と根拠

ORDレコード
ord-854c51b8d09f40c48d3a03ca81d923d3
出典データセット
uspto-grants-2012_06
特許番号
US08193184B2

関連ノート

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