Ammonia → HCID 21200669、化合物

HRID 1066539ノート

反応式

HRID 1066539 の反応式
[CH3:1][C:2]1([CH3:11])[CH:7]([OH:8])[CH:6]([CH3:9])[CH2:5][C:4](=O)[CH2:3]1.C([O-])(=O)C.[NH4+:16].N.[H][H]>CO.[Ni]>[NH2:16][CH:4]1[CH2:5][CH:6]([CH3:9])[CH:7]([OH:8])[C:2]([CH3:11])([CH3:1])[CH2:3]1

参加物

7

反応物 4

HCID 222AmmoniaHCID 517165Ammonium AcetateHCID 212006704-Hydroxy-3,3,5-trimethylcyclohexanoneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 21200669HCID 21200669、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

156 g of 3,3,5-trimethyl-4-hydroxycyclohexanon (formula VIa), 12 g of ammonium acetate and 60 g of Raney Ni in 250 ml methanol were hydrogenated at 100° C. under a hydrogen pressure of 100 bar in the presence of 250 ml of ammonia. When the uptake of hydrogen was complete, the catalyst was filtered off, the filtrate was concentrated under vacuum and the residue was subjected to fractional distillation under a high vacuum. 130 g of the aminoalcohol of formula Ic, which had a melting point of 110 to 112° C., were obtained at 90 to 97° C. (0.1 mbar). According to analysis by gas chromatography, an isomer mixture (four isomers) was present.

後処理

  1. customwere hydrogenated at 100° C. under a hydrogen
  2. filtrationthe catalyst was filtered off
  3. concentrationthe filtrate was concentrated under vacuum
  4. distillationthe residue was subjected to fractional distillation under a high vacuum
  5. customwere obtained at 90 to 97° C. (0.1 mbar)

出典と根拠

ORDレコード
ord-95463e942bad43e6a61808a51dd2f6b4
出典データセット
uspto-grants-2001_06
特許番号
US06242641B1

反応ノート

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