Ammonia → HCID 21200669, 화합물

HRID 1066539노트

반응식

HRID 1066539 반응식
[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

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 517165Ammonium AcetateHCID 212006704-Hydroxy-3,3,5-trimethylcyclohexanoneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 21200669HCID 21200669, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-95463e942bad43e6a61808a51dd2f6b4
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242641B1

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