反応式
[CH:1]1([C:4]([OH:6])=[O:5])[CH2:3][CH2:2]1.[CH:7]1([C:10]([Cl:12])=[O:11])[CH2:9][CH2:8]1.Cl.O[CH:15]([C:30]1[CH:39]=[CH:38][C:37]([OH:40])=[C:36]2[C:31]=1[CH:32]=[CH:33][C:34](=[O:41])[NH:35]2)[CH2:16][NH:17][CH2:18][CH2:19][C:20]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[C:22]([O:28][CH3:29])[CH:21]=1.CO>C(OCC)C>[ClH:12].[CH:1]1([C:4]([O:6][CH:15]([C:30]2[CH:39]=[CH:38][C:37]([O:40][C:10]([CH:7]3[CH2:9][CH2:8]3)=[O:11])=[C:36]3[C:31]=2[CH:32]=[CH:33][C:34](=[O:41])[NH:35]3)[CH2:16][NH:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[C:22]([O:28][CH3:29])[CH:21]=2)=[O:5])[CH2:3][CH2:2]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
2 ml of cyclopropanecarboxylic acid and 1 ml of cyclopropanecarboxylic acid chloride were added to 500 mg of 5-[1-hydroxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-hydroxycarbostyril hydrochloride, and the mixture was allowed to react for 1 hour at a temperature of 80° C. After completion of the reaction, 10 ml of methanol was added to the reaction mixture while cooling with ice-water followed by addition of diethyl ether to crystallize the product. The crystals thus obtained were separated by filtration, washed with diethyl ether and recrystallized from a mixture of ethanol and acetone to obtain 210 mg of 5-[1-cyclopropylcarbonyloxy-2-(3,4-dimethoxyphenethylamino)ethyl]-8-cyclopropylcarbonyloxycarbostyril hydrochloride having a melting point of 167°-168° C. (with decomposition).
後処理
- customto react for 1 hour at a temperature of 80° C
- additionwas added to the reaction mixture
- customto crystallize the product
- customThe crystals thus obtained
- customwere separated by filtration
- washwashed with diethyl ether
- customrecrystallized from a mixture of ethanol and acetone
出典と根拠
- ORDレコード
- ord-8294f87b96c34758a9476c5d5ebb2992
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04223137
関連ノート
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