Sodium Dithionite → 5-bromo-N4-ethylpyridine-3,4-diamine
反応式
[Br:1][C:2]1[C:3]2[N:10](CC)[C:9]([C:13]3C(N)=NON=3)=[N:8][C:4]=2[CH:5]=[N:6][CH:7]=1.S(S([O-])=O)([O-])=O.[Na+].[Na+]>C(O)C.O.ClCCl>[Br:1][C:2]1[C:3]([NH:10][CH2:9][CH3:13])=[C:4]([NH2:8])[CH:5]=[N:6][CH:7]=1参加物
6
実験手順
A solution of the product of Step 1 (0.5 g, 2 mmol) in ethanol (8 ml)/water (10 ml) was stirred at 60° C. and sodium dithionite (2.12 g, 12.2 mmol) was added protionwise. After 10 minutes the mixture was cooled to room temperature, and diluted with water and dichloromethane. The organic phase was dried and evaporated in vacuo, the residue was used directly in the next reaction; 1H NMR (DMSO-d6) 7.76 (1H, s), 7.75 (1H, s), 5.0 (2H, br), 4.46 (1H, t, J=9.6 Hz), 3.26 (2H, m), 1.06 (3H, t, J=7.2 Hz).
後処理
- customThe organic phase was dried
- customevaporated in vacuo
- customthe residue was used directly in the next reaction
出典と根拠
- ORDレコード
- ord-5702a78cb4e9455da3f029b1ab817159
- 出典データセット
- uspto-grants-2008_03
- 特許番号
- US07348339B2
反応ノート
読み込み中…