Hydrogen Bromide → Undecane hydrobromide
反応式
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[BrH:12]>C(O)(=O)C>[BrH:12].[CH3:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1]参加物
4
実験手順
D,L-2-aza-2'-hydroxy-5,6-benzotricyclo[6.3.01,8.04,11 ] undecane (2.68 g; 11.7 mmoles) is refluxed under argon in a mixture of acetic acid (67 ml) and 47% hydrobromic acid (677 ml) for 30 hours. The mixture is evaporated to dryness. The residue is dissolved in hot methanol and evaporated onto 15 g silica gel which is then placed on top of 80 g silica gel. Elution with chloroform:methanol:ammonium hydroxide (100:15:1 v:v:v) yields D,L-2-aza-2'-hydroxy-5,6-benzotricyclo[6.3.01,8.04,11 ] undecane hydrobromide: 2.23 g, 89%; melting point: 284°-286° C.
後処理
- customThe mixture is evaporated to dryness
- dissolutionThe residue is dissolved in hot methanol
- customevaporated onto 15 g silica gel which
- washElution with chloroform:methanol:ammonium hydroxide (100:15:1 v:v:v)
出典と根拠
- ORDレコード
- ord-ad3f8c104c4344c8982320022ee490e6
- 出典データセット
- uspto-grants-1983_03
- 特許番号
- US04376779
反応ノート
読み込み中…