8-Benzyloxy-6-methoxymethyl-2,3-dimethylimidazo[1,2-a]pyridine → 6-Methoxymethyl-2,3-dimethyl-5,6,7,8-tetrahydroimidazo[1,2-a]pyridin-8-one
反応式
C([O:8][C:9]1[C:10]2[N:11]([C:18]([CH3:22])=[C:19]([CH3:21])[N:20]=2)[CH:12]=[C:13]([CH2:15][O:16][CH3:17])[CH:14]=1)C1C=CC=CC=1.[H][H]>CO.[Pd]>[CH3:17][O:16][CH2:15][CH:13]1[CH2:12][N:11]2[C:18]([CH3:22])=[C:19]([CH3:21])[N:20]=[C:10]2[C:9](=[O:8])[CH2:14]1参加物
5
実験手順
19.2 g of 8-benzyloxy-6-methoxymethyl-2,3-dimethylimidazo[1,2-a]pyridine, dissolved in 100 ml of methanol, are treated with 1.9 g of palladium (10% strength on activated carbon, Merck) and hydrogenated with hydrogen at 80° C. using a pressure of 50 bar. After absorption of hydrogen is complete, the catalyst is filtered off, washed with methanol and methylene chloride and the combined filtrate is concentrated to dryness in vacuo. After purification on silica gel (eluent: methylene chloride/methanol=13/1), 7.6 g of the title compound of melting point 103-104° C. are obtained.
後処理
- customAfter absorption of hydrogen
- filtrationthe catalyst is filtered off
- washwashed with methanol and methylene chloride
- concentrationthe combined filtrate is concentrated to dryness in vacuo
- customAfter purification on silica gel (eluent: methylene chloride/methanol=13/1), 7.6 g of the title compound of melting point 103-104° C.
- customare obtained
出典と根拠
- ORDレコード
- ord-872f340cf1af4aca9370b7461bc970d1
- 出典データセット
- uspto-grants-2005_03
- 特許番号
- US06869949B2
反応ノート
読み込み中…