反応式
Cl.[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([CH2:20][C:21]([OH:23])=[O:22])=[CH:16][CH:15]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1.C(C1NC=CN=1)(C1NC=CN=1)=O.[NH2:36][CH:37]1[CH2:42][CH2:41][CH2:40][N:39]([CH2:43][CH3:44])[CH2:38]1.O>CS(C)=O>[OH2:22].[Cl:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([NH:13][C:14]3[CH:15]=[CH:16][C:17]([CH2:20][C:21]([NH:36][CH:37]4[CH2:42][CH2:41][CH2:40][N:39]([CH2:43][CH3:44])[CH2:38]4)=[O:23])=[CH:18][CH:19]=3)=[CH:8][CH:9]=[N:10]2)=[CH:5][CH:4]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 100 °C
実験手順
7.0 Grams (0.02 mole) of 2-[4-(7-chloro-4-quinolylamino)phenyl]acetic acid hydrochloride were dissolved in 150 milliliters of dimethyl sulphoxide by heating the stirred mixture to 100° C. under nitrogen. The solution was cooled to room temperature, 6.48 grams (0.04 mole) of carbonyl di-imidazole were added and the mixture was stirred for 21/2 hours under nitrogen. 7.68 Grams (0.06 mole) of 3-amino-1-ethylpiperidine were added, the solution was stirred for another 21/2 hours and poured into 500 milliliters of water. The mixture was refrigerated overnight and the resulting solid was broken up, stirred with water, collected and dried. The solid was dissolved in chloroform and chromatographed on an alumina column made up in chloroform. Elution with chloroform/methanol (4:1) gave 8.15 grams (92.5% yield) of 2-[4-(7-chloro-4-quinolylamino)phenyl]-N-(1-ethyl-3-piperidyl)acetamide monohydrate, melting point 160°-162° C.
後処理
- temperatureThe solution was cooled to room temperature
- stirringthe solution was stirred for another 21/2 hours
- waitThe mixture was refrigerated overnight
- customcollected
- customdried
- dissolutionThe solid was dissolved in chloroform
- customchromatographed on an alumina column
- washElution with chloroform/methanol (4:1)
出典と根拠
- ORDレコード
- ord-eb994b99a963498aa299fb5d018646e3
- 出典データセット
- uspto-grants-1980_11
- 特許番号
- US04235908
関連ノート
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