反応式
C(S)(=N)N.[NH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.[C:11]([NH2:15])(=[O:14])[CH:12]=[CH2:13]>CCO>[N:5]1([CH2:13][CH2:12][C:11]([NH2:15])=[O:14])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1参加物
5
実験手順
Carbamimidothioic acid, N'-cyano-N-[3-[4-(diphenylmethylene)-1-piperidinyl]-propyl]-, methyl ester. A solution of piperidine, 4-(diphenylmethylene) (0.10 mole) and acrylamide (8.95 g, 0.062 mole) in EtOH (50 ml) was refluxed overnight. This reaction mixture was filtered and concentrated. The resulting while solid residue was dissolved in CHCl3, washed with H2O (3×150 ml), dried (Na2SO4) and the solvent removed to give thick yellow oil. Crystallization from CH2Cl2 -i-Pr2O afforded 29.01 g (75%) of 1-piperidinepropanamide, 4-(diphenylmethylene)-; mp 105°-7° C.
後処理
- filtrationThis reaction mixture was filtered
- concentrationconcentrated
- dissolutionThe resulting while solid residue was dissolved in CHCl3
- washwashed with H2O (3×150 ml)
- dry with materialdried (Na2SO4)
- customthe solvent removed
- customto give thick yellow oil
- customCrystallization from CH2Cl2 -i-Pr2O
出典と根拠
- ORDレコード
- ord-1789272e3d394ccf8937f1b06bce883b
- 出典データセット
- uspto-grants-1986_04
- 特許番号
- US04584301
関連ノート
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