反応式
[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][NH2:6])[CH3:2].[C:9](N1C=CN=C1)(N1C=CN=C1)=[O:10].[CH3:21][CH:22]([NH:24][CH:25]([CH3:36])[CH2:26][S:27]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)(=[O:29])=[O:28])[CH3:23]>O1CCCC1>[OH2:10].[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][NH:6][C:9](=[O:10])[N:24]([CH:22]([CH3:21])[CH3:23])[CH:25]([CH3:36])[CH2:26][S:27]([C:30]1[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1)(=[O:28])=[O:29])[CH3:2]参加物
5
実験手順
A solution of 3.71 g (0.032 mole) of N,N-diethylethylenediamine and 5.83 (0.036 mole) of 1,1'-carbonyldiimidazole in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 8.30 g (0.030 mole) of N-(2-propyl)-1-(phenylsulfonyl)-2-propanamine in 50 ml of tetrahydrofuran was added and the solution was refluxed overnight. The solvent was removed in vacuo, and the residue was partitioned between ether and water. The ether solution was dried over magnesium sulfate and the solvent was removed in vacuo to give an oil. The oil was flash chromatographed (silica gel; elution with methanol) to give an oil. Crystallization from ether gave 0.54 g (4.5%) of white, crystalline solid, m.p. 75°-80° C.
後処理
- temperaturethe solution was refluxed overnight
- customThe solvent was removed in vacuo
- customthe residue was partitioned between ether and water
- dry with materialThe ether solution was dried over magnesium sulfate
- customthe solvent was removed in vacuo
- customto give an oil
- customchromatographed
- wash(silica gel; elution with methanol)
- customto give an oil
- customCrystallization from ether
- customgave 0.54 g (4.5%) of white, crystalline solid, m.p. 75°-80° C.
出典と根拠
- ORDレコード
- ord-f16b105db12b494fba7b6c0c4a34a623
- 出典データセット
- uspto-grants-1986_07
- 特許番号
- US04597902
関連ノート
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