Dichloromethane → 3-Azido-5-isopropyl-azepan-2-one
反応式
Cl[CH:2]1[CH2:8][CH:7]([CH:9]([CH3:11])[CH3:10])[CH2:6][CH2:5][NH:4][C:3]1=[O:12].[N-:13]=[N+:14]=[N-:15].[Na+].C(Cl)Cl>CS(C)=O.O>[N:13]([CH:2]1[CH2:8][CH:7]([CH:9]([CH3:11])[CH3:10])[CH2:6][CH2:5][NH:4][C:3]1=[O:12])=[N+:14]=[N-:15]参加物
6
実験手順
3-Chloro-5-isopropyl-azepan-2-one (3.4 g, 18 mmol) and sodium azide (3.51 g, 53.9 mmol) were reacted in dry dimethyl sulfoxide (50 ml) overnight at 80° C. under an argon atmosphere. The reaction mixture was allowed to cool to r.t. diluted with water (200 ml) and extrated with CH2Cl2 (4×). The combined organic fractions were washed with water (3×), brine and dried (MgSO4) filtered and evaporated under reduced pressure. The crude yellow oil was purified over silica gel (ethyl acetate/n-heptane 1:2): yellow oil 2.6 g (70%); MS: m/e=197.4 (MH+)
後処理
- washThe combined organic fractions were washed with water (3×), brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated under reduced pressure
- customThe crude yellow oil was purified over silica gel (ethyl acetate/n-heptane 1:2)
出典と根拠
- ORDレコード
- ord-5878004b8cc6455e8d7866e4885c3d29
- 出典データセット
- uspto-grants-2007_08
- 特許番号
- US07253158B2
反応ノート
読み込み中…