Hydrochloric Acid → (4-Methoxy-6-methylpyrimidin-2-YL)methanamine
反応式
[C:1]([C:3]1[N:8]=[C:7]([CH3:9])[CH:6]=[C:5]([O:10][CH3:11])[N:4]=1)#[N:2].Cl>[Pd].CO>[NH2:2][CH2:1][C:3]1[N:8]=[C:7]([CH3:9])[CH:6]=[C:5]([O:10][CH3:11])[N:4]=1参加物
5
実験手順
A mixture of 4.4 g of the product from Example 8, 0.35 g 10% palladium-on-carbon catalyst, and 1.5 ml of concentrated hydrochloric acid in 70 ml methanol was shaken under an atmosphere of hydrogen at 46 p.s.i. on a Parr Hydrogenation Apparatus. After 31/2 hours, the solution was filtered through a pad of Celite and the filtrate was concentrated in vacuo. The resulting solid was taken up in water and the aqueous layer was washed with several small portions of ether. Adjustment to pH 13 followed by extraction with methylene chloride, drying, and evaporation of the organic layer gave 1.8 g of the title compound as a light yellowish-orange oil.
後処理
- filtrationAfter 31/2 hours, the solution was filtered through a pad of Celite
- concentrationthe filtrate was concentrated in vacuo
- washthe aqueous layer was washed with several small portions of ether
- extractionfollowed by extraction with methylene chloride
- customdrying
- customevaporation of the organic layer
出典と根拠
- ORDレコード
- ord-19b7e2eb7f3d4cca8d3f6735446723d3
- 出典データセット
- uspto-grants-1986_01
- 特許番号
- US04565567
反応ノート
読み込み中…