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

HRID 745665

反応式

HRID 745665 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f1561701e6b24ec198473128bf3b15cf
出典データセット
uspto-grants-1986_07
特許番号
US04599420

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