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Ammonia → 2,6-Dimethylcyclohexylamine

HRID 2296501
ノート
印刷プレビュー

反応式

HRID 2296501 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1O.[O-2].[Pr+3].[O-2].[O-2].[Pr+3].[O-2].[Al+3].[O-2].[O-2].[Al+3].[NH3:20]>[H][H].[Pd]>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH:4]([CH3:8])[CH:3]1[NH2:20]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 222AmmoniaHCID 113352,6-DimethylphenolHCID 165911Praseodymium oxideHCID 9989226Alumina

生成物 1

HCID 1109322,6-Dimethylcyclohexylamine収率 99.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 178418361
HCID 178418361、化合物
溶媒

反応条件

温度
230 °C

実験手順

1.650 kg of 2,6-dimethylphenol and 150 g of a pulverulent catalyst which contains 5.0% by weight of palladium and 2.5% by weight of praseodymium oxide, the remainder being aluminum oxide, are introduced into a 10 l stirred autoclave. The autoclave is closed and 1.370 kg of ammonia are forced in. The mixture is then heated to 230° C. and a pressure of 200 bar is established by forcing in hydrogen. The mixture is kept at the reaction temperature until a constant pressure is achieved (about 8 hours). It is then left to cool, and is filtered to give 1.710 kg of crude 2,6-dimethylcyclohexylamine (a mixture of 3 stereoisomeric 2,6-dimethylcyclohexylamines). The crude product is distilled to give 1.685 kg of 2,6-dimethylcyclohexylamine, boiling point=167°-168° C., corresponding to a yield of 98%.

後処理

  1. additionare introduced into a 10 l
  2. customThe autoclave is closed
  3. custom(about 8 hours)
  4. waitIt is then left
  5. temperatureto cool
  6. filtrationis filtered

出典と根拠

ORDレコード
ord-88a026750b744c7c9ed03bcef7aacd3f
出典データセット
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04429155

反応ノート

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