Ammonium Acetate → 9-Methyl-9-azabicyclo(3.3.1)nonan-3-amine

HRID 247159

반응식

HRID 247159 반응식
[CH3:1][N:2]1[CH:7]2[CH2:8][CH2:9][CH2:10][CH:3]1[CH2:4][C:5](=[N:11]O)[CH2:6]2.C([O-])(=O)C.[NH4+]>C(O)C.[Ni]>[NH2:11][CH:5]1[CH2:4][CH:3]2[N:2]([CH3:1])[CH:7]([CH2:8][CH2:9][CH2:10]2)[CH2:6]1

참가 물질

5

반응물 2

HCID 517165Ammonium AcetateHCID 32191339-Methyl-9-azabicyclo[3.3.1]nonan-3-one oxime

생성물 1

HCID 144031759-Methyl-9-azabicyclo(3.3.1)nonan-3-amine수율 90%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

N-methyl-9-azabicyclo-[3.3.1]-nonan-3-one oxime (3.25 g., 0.02 mole) was dissolved in ethanol and hydrogenated over Raney nickel in the presence of ammonium acetate at 300 p.s.i. at 50° C. for 24 hours. The mixture was filtered, evaporated in vacuo, dissolved in dilute hydrochloric acid, basified and extracted into ethyl acetate. The combined organic layers were dried (K2CO3), filtered and evaporated in vacuo to yield 3-amino-9-methyl-9-azabicyclo-[3.3.1]-nonane (2.67 g., 90%), used without further purification.

후처리

  1. filtrationThe mixture was filtered
  2. customevaporated in vacuo
  3. dissolutiondissolved in dilute hydrochloric acid
  4. extractionextracted into ethyl acetate
  5. dry with materialThe combined organic layers were dried (K2CO3)
  6. filtrationfiltered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-93a3afc5e7c94dd0a40f78baf4e0daac
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705858

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