HCID 242258, 화합물 → Tricyclo(5.2.1.0,2,6)decan-8-amine

HRID 2416993

반응식

HRID 2416993 반응식
[CH2:1]1[CH:9]2[CH:4]([CH:5]3[CH2:10][CH:8]2[CH2:7][C:6]3=[N:11]O)[CH:3]=[CH:2]1>CO.[Ni].O>[CH2:1]1[CH:9]2[CH:4]([CH:5]3[CH2:10][CH:8]2[CH2:7][CH:6]3[NH2:11])[CH2:3][CH2:2]1

참가 물질

5

실험 절차

2.2 g of 1,3a,4,6,7,7a-hexahydro-4,7-methanoinden-5-one oxime were dissolved in 50 ml of methanol, and about 10% Raney nickel, dissolved in 50% water, was added. The mixture was hydrogenated at 100 bar and 100° C. for 20 hours, the catalyst was then filtered off, and the solvent was evaporated under reduced pressure. The residue was taken up in ether and 6 N aqueous sodium hydroxide solution, the phases were separated, the aqueous phase was extracted three times with ether, the combined organic phases were dried with magnesium sulfate and filtered, and the filtrate was concentrated. This gave 1.8 g of a colorless oil which was purified by kugelrohr distillation. This gave 0.96 g of the desired amine as an oil.

후처리

  1. additionwas added
  2. filtrationthe catalyst was then filtered off
  3. customthe solvent was evaporated under reduced pressure
  4. custom6 N aqueous sodium hydroxide solution, the phases were separated
  5. extractionthe aqueous phase was extracted three times with ether
  6. dry with materialthe combined organic phases were dried with magnesium sulfate
  7. filtrationfiltered
  8. concentrationthe filtrate was concentrated
  9. distillationThis gave 1.8 g of a colorless oil which was purified by kugelrohr distillation

출처 및 근거

ORD 기록
ord-a5c67892925548bbac54c7dace066cc8
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825231B2

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