Ammonia → 3,4-Diethoxyphenethylamine

HRID 1704235ノート

反応式

HRID 1704235 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[O:13][CH2:14][CH3:15])[CH2:7][C:8]#[N:9])[CH3:2].N>[Ni].C(O)C>[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH2:7][CH2:8][NH2:9])[CH:10]=[CH:11][C:12]=1[O:13][CH2:14][CH3:15])[CH3:2]

参加物

5

反応物 2

HCID 222AmmoniaHCID 520318(3,4-Diethoxyphenyl)acetonitrile

生成物 1

HCID 8406943,4-Diethoxyphenethylamine

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

100 kg. of 3,4-diethoxy-benzyl cyanide are hydrogenated in 310 1. of a 80 to 96% aqueous ethanol containing 9 to 12% of ammonia in the presence of 24 kg. of a Raney-nickel catalyst pretreated according to Example 3, at 45° to 68° C under a hydrogen overpressure of 8 to 10 atm. The catalyst is filtered off, the solution is evaporated and the residue is subjected to fractionation in vacuo. Thus 96 kg. of highly pure 3,4-diethoxy-beta-phenyl-ethylamine are obtained. The purity is almost 100%. The mono-desethylated beta-phenyl-ethylamine derivative is present at most in traces in such a small amount, which can not be detected by thin layer chromatography.

後処理

  1. custompretreated according to Example 3, at 45° to 68° C under a hydrogen overpressure of 8 to 10 atm
  2. filtrationThe catalyst is filtered off
  3. customthe solution is evaporated

出典と根拠

ORDレコード
ord-5cb0b8e7e8524b28afe2651f597e5194
出典データセット
uspto-grants-1978_11
特許番号
US04126615

反応ノート

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