反応式
F[C:2](F)(F)[C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[N:12]=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1.[Na]>C(O)(=O)C>[CH3:2][C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[NH:12][CH2:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1参加物
4
実験手順
7-[3-Methylphenyl)pyrazolo[1,5-a]pyrimidine-3-carboxamine (prepared as described in Example 1) is stirred as a suspension in gacial acetic acid (cooled in an ice bath) under nitrogen and then excess sodium cyanoborohydide is added to the reaction mixture in portions. After one hour of stirring in the ice bath, the mixture is stirred at room temperature for 19 hours. This solution is evaporated to dryness, then water is added and the white precipitate which forms is collected by filtration and washed with an aqueous saturated solution of sodium bicarbonate, and finally with water. The solid is collected by filteration and dried to give 4,5-dihydro-7-(3-methylphenyl)pyrazolo[1,5-a]pyrimidine-3-carboxamide.
後処理
- customThis solution is evaporated to dryness
- additionwater is added
- filtrationthe white precipitate which forms is collected by filtration
- washwashed with an aqueous saturated solution of sodium bicarbonate
- customThe solid is collected by filteration
- customdried
出典と根拠
- ORDレコード
- ord-13273e52e29d4e92b3d25db03243337d
- 出典データセット
- uspto-grants-1990_04
- 特許番号
- US04916137
関連ノート
読み込み中…