反応式
[CH2:1]1[CH:8]2[C:4]3([C:10]([OH:12])=[O:11])[CH2:5][CH:6]([CH2:9][CH:2]1[CH2:3]3)[CH2:7]2.C(N1C=CN=C1)(N1C=CN=C1)=O.C(=O)=O.[CH3:28][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[N:36]1[CH2:41][CH2:40][N:39]([CH2:42][CH2:43][CH2:44]O)[CH2:38][CH2:37]1>C(Cl)(Cl)Cl>[CH3:28][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[N:36]1[CH2:37][CH2:38][N:39]([CH2:42][CH2:43][CH2:44][O:11][C:10]([C:4]23[CH2:5][CH:6]4[CH2:9][CH:2]([CH2:1][CH:8]2[CH2:7]4)[CH2:3]3)=[O:12])[CH2:40][CH2:41]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a stirred solution of hexahydro-2,5-methanopentalene-3a[1H]-carboxylic acid (0.6 g, 3.6×10-3 mol) in 25 ml of chloroform under a dry nitrogen atmosphere was added carbonyldiimidazole (0.58 g, 3.6×10-3 mol). The resulting solution was stirred at ambient temperature for three hours, during which time a gas (CO2) was evolved. A solution of 3-[1-(2-methoxyphenyl)-4-piperazinyl]propanol (0.91 g, 3.6×10-3 mol) in 25 ml of chloroform was then added, and the resulting reaction mixture was stirred under nitrogen at ambient temperature for two days. The mixture was diluted to 150 ml with chloroform, washed with three-one hundred ml portions of water, dried over anhydrous sodium sulfate, and concentrated on a rotary evaporator. The desired product (TLC on silica using a 30% methanol in ethyl acetate solvent system, Rf=0.52) was isolated by gravity chromatography on silica gel and converted to the hydrochloride salt with isopropanolic HCl (0.84 g, 50% yield), mp.=206°-207° C.
後処理
- customthe resulting reaction mixture
- washwashed with three-one hundred ml portions of water
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated on a rotary evaporator
出典と根拠
- ORDレコード
- ord-8eb5d609223f459f83e97bd528335418
- 出典データセット
- uspto-grants-1989_10
- 特許番号
- US04873331
関連ノート
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