氨 → 内向-3-氨基-9-甲基-9-氮杂双环[3,3,1]壬烷

HRID 341943

反应方程式

HRID 341943 反应方程式
[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.N>CO>[CH3:1][N:2]1[C@@H:7]2[CH2:6][CH:5]([NH2:11])[CH2:4][C@H:3]1[CH2:10][CH2:9][CH2:8]2

参与物

4

反应物 2

HCID 222氨HCID 3219133高托品酮肟

产物 1

HCID 11008150内向-3-氨基-9-甲基-9-氮杂双环[3,3,1]壬烷收率 93%

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

A solution of 9-methyl-9-azabicyclo[3.3.1]nonan-3-one oxime (10 g, 0.06 moles) in methanol (70 ml) and 0.88 ammonia; (36 ml; 10.0 equivs) was hydrogenated at 50° C. and 50 psi (344.8 kPa)/H2 for 16 hrs using 5% Rhodium on carbon paste (1 g dry weight). The reaction mixture was cooled to room temperature and filtered to remove catalyst. The catalyst bed was washed with methanol and the methanolic solution was then evaporated under reduced pressure to give the title compound as an oil (8.6 g, 93% weight recovery) which solidified to a waxy solid on standing (8.6 g, 93%).

后处理

  1. customwas hydrogenated at 50° C.
  2. dry with material5% Rhodium on carbon paste (1 g dry weight)
  3. filtrationfiltered
  4. customto remove catalyst
  5. washThe catalyst bed was washed with methanol
  6. customthe methanolic solution was then evaporated under reduced pressure

来源与证据

ORD记录
ord-cc0d3a87311340899db2f5ecccf0561d
来源数据集
uspto-grants-1999_01
专利号
US05856489

关联笔记

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