Potassium Hydroxide → HCID 117667602、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[NH:8][CH2:7][CH2:6][CH2:5]2.ClC(Cl)(Cl)[C:14]([N:16]=C=O)=[O:15].[OH-].[K+]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[N:10][CH:11]=1)[N:8]([C:14]([NH2:16])=[O:15])[CH2:7][CH2:6][CH2:5]2参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a cooled (0° C.) solution of 6-bromo-1,2,3,4-tetrahydro-[1,8]naphthyridine (6.4 g, 30.0 mmol) in DCM (75 mL) is added a trichloroacetyl isocyanate (3.8 mL, 31.5 mmol). After stirring for 1 h at 0° C., a solution of methanolic KOH (1M, 10 mL) is added. The resulting mixture is allowed to warm and stir at room temperature for 16 h. The reaction is concentrated and purified by silica gel column (0-100% EtOAc in heptane) to afford the title compound (7.4 g).
後処理
- temperatureto warm
- stirringstir at room temperature for 16 h
- concentrationThe reaction is concentrated
- custompurified by silica gel column (0-100% EtOAc in heptane)
出典と根拠
- ORDレコード
- ord-10fb7eb43d054d6da54d6dc2c3f65a8e
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181272B2
反応ノート
読み込み中…