反応式
[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([O:16][CH3:17])[C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([Cl:18])[N:3]=1.[NH:19]1[CH2:24][CH2:23][CH:22]([N:25]2[C:34](=[O:35])[CH2:33][C:28]3([CH2:32][CH2:31][CH2:30][CH2:29]3)[CH2:27][C:26]2=[O:36])[CH2:21][CH2:20]1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[ClH:18].[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([O:16][CH3:17])[C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:19]2[CH2:24][CH2:23][CH:22]([N:25]3[C:26](=[O:36])[CH2:27][C:28]4([CH2:32][CH2:31][CH2:30][CH2:29]4)[CH2:33][C:34]3=[O:35])[CH2:21][CH2:20]2)[N:3]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
The mixture of 5.39 g of 4-amino-2-chloro-6,7,8-trimethoxyquinazoline, 5.25 g of 8-(4-piperidinyl)-8-azaspiro-[4,5]decan-7,9-dione, 4.24 g of anhydrouus sodium carbonate and 75 ml of dimethylformamide is stirred at 150° for 8 hours. After cooling to room temperature it is filtered, the filtrate evaporated, the residue dissolved in ethyl acetate and the solution washed with aqueous sodium bicarbonate and water. It is dried, evaporated, the residue dissolved in 75 ml of ethyl acetate and allowed to crystallize. The crystals are dissolved in 50 ml of hot isopropanol and the solution acidified with hydrogen chloride to pH=1 and the precipitate filtered off, to yield the 8-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-8-azaspiro[4,5]decan-7,9dione monohydrochloride melting at 225°-227°.
後処理
- filtrationis filtered
- customthe filtrate evaporated
- dissolutionthe residue dissolved in ethyl acetate
- washthe solution washed with aqueous sodium bicarbonate and water
- customIt is dried
- customevaporated
- dissolutionthe residue dissolved in 75 ml of ethyl acetate
- customto crystallize
- dissolutionThe crystals are dissolved in 50 ml of hot isopropanol
- filtrationthe precipitate filtered off
出典と根拠
- ORDレコード
- ord-2cf195942baf4d168b10694f110acb88
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04255429
関連ノート
読み込み中…