Ammonium Hydroxide → 1-Propanamine, 3-butoxy-

HRID 1770243ノート

反応式

HRID 1770243 の反応式
C(OC(C)C#N)CCC.C(O)C.[OH-].[NH4+].[OH-].[NH4+].[CH2:17]([O:21][CH:22](OCCCC)[CH2:23][CH2:24][NH2:25])[CH2:18][CH2:19][CH3:20]>[Ni]>[CH2:17]([O:21][CH2:22][CH2:23][CH2:24][NH2:25])[CH2:18][CH2:19][CH3:20]

参加物

6

反応物 4

HCID 14923Ammonium HydroxideHCID 19069539DibutoxypropylamineHCID 20095850ButoxypropionitrileHCID 22731726Ethanol ammonium hydroxide

生成物 1

HCID 854611-Propanamine, 3-butoxy-収率 79.5%

試薬・触媒・溶媒 1

HCID 935Nickel触媒

反応条件

温度
60 °C

実験手順

The previously prepared butoxypropionitrile (224.8 grams) was combined with Raney nickel (20 grams of 50/50 mixture with water) in a 1-liter stainless steel autoclave along with a premixed ethanol/ammonium hydroxide solution (37.5 grams of ammonium hydroxide and 212.5 grams of ethanol). The addition of the ammonium hydroxide limits the reaction that leads to the formation of by-product dibutoxypropylamine. After purging with nitrogen, the reactor was pressurized with 500 psi of hydrogen and heated to 60° C. After 20 hours at this temperature, the reactor was cooled to room temperature and the product discharged. The product was filtered to remove the Raney nickel and then distilled using a simple Vigreux column to extract the butoxypropylamine. The distillation produced a yield of about 79.5% of product and 18.3% of the secondary amine.

後処理

  1. customthe reaction that
  2. customAfter purging with nitrogen
  3. temperaturethe reactor was cooled to room temperature
  4. filtrationThe product was filtered
  5. customto remove the Raney nickel
  6. distillationdistilled
  7. extractionto extract the butoxypropylamine
  8. distillationThe distillation

出典と根拠

ORDレコード
ord-886ea6d7f9604e5fa53bb0dc3bd6edd2
出典データセット
uspto-grants-1995_01
特許番号
US05385948

反応ノート

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