Ammonia → 6-Aminohexanenitrile

HRID 1954487ノート

反応式

HRID 1954487 の反応式
[CH:1]([CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[N:8])=O.[NH3:9]>[H][H]>[NH2:9][CH2:1][CH2:3][CH2:4][CH2:5][CH2:6][C:7]#[N:8].[NH2:9][CH2:1][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH2:8]

参加物

5

反応物 2

HCID 222AmmoniaHCID 110406526-Oxohexanenitrile

生成物 2

HCID 16402Hexamethylenediamine収率 12%HCID 170796-Aminohexanenitrile収率 73%

試薬・触媒・溶媒 1

HCID 178418361HCID 178418361、化合物溶媒2 回

反応条件

温度
80 °C

実験手順

In an autoclave having a capacity of 300 ml and equipped with a sampling sluice (material HC 4) there were placed 11 g of 5-formylvaleronitrile and 3 g of Ru (3%) on Al2O3 (4 mm extrudates) under protective gas (argon). The autoclave was then sealed and 150 ml of NH3 were forced in. Thorough mixing was effected using a magnetic stirrer. After heating to 80° C. (autogenous pressure: ca. 39 bar) the mixture was kept at 80° C. for a further 2 hours and then the overall pressure was raised, with hydrogen, to 70 bar. The pressure of 70 bar was maintained by constantly forcing in more hydrogen. After 25 hours, the autoclave was depressurized and the hydrogenation effluent analyzed by gas chromatography. The products formed comprised 73% of 6-aminocapronitrile and 12% of hexamethylene diamine. The conversion was 100%.

後処理

  1. customequipped with a sampling sluice (material HC 4) there
  2. customThe autoclave was then sealed
  3. additionThorough mixing
  4. temperatureThe pressure of 70 bar was maintained
  5. waitAfter 25 hours

出典と根拠

ORDレコード
ord-63d24e8db18247ac85c4af57ca8484bc
出典データセット
uspto-grants-2000_09
特許番号
US06121481

反応ノート

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