反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:13][CH:12]([CH2:14]N3CCN(C(C(OCC)=O)CC(OCC)=O)CC3)[O:11][C:10]2=[O:33])=[CH:5][CH:4]=1)#[N:2].C(C1C=CC(N)=CC=1)#N.[O:43]1CC1CO.C(C1C=CC(NCC(O)CO)=CC=1)#N.C(=O)(OCC)OCC.CC(C)([O-])C>>[C:1]([C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:13][CH:12]([CH2:14][OH:43])[O:11][C:10]2=[O:33])=[CH:7][CH:8]=1)#[N:2]参加物
実験手順
1.3 g of 3-(4-cyanophenyl)-5-[4-(1,2-diethoxycarbonylethyl)piperazinomethyl)oxazolidin-2-one [obtainable by reaction of 4-cyanoaniline with 2,3-epoxypropan-1-ol to give N-[4-cyanophenyl]-2,3-dihydroxypropylamine, reaction with diethyl carbonate in the presence of K tert-butoxide to give 3-(4-cyano-phenyl)-5-hydroxymethyloxazolidin-2-one, subsequent esterification with methanesulfonyl chloride and reaction with "B"] and 1.1 g of hydroxylamine hydrochloride are boiled for 2 hours in 125 ml of ethanol in the presence of 2.24 g of sodium ethoxide. The reaction mixture is then filtered and concentrated in vacuo. The residue is dissolved in water, the solution is adjusted to pH 3 using 2N hydrochloric acid and the resulting precipitate is filtered off with suction. After recrystallizing from water/glacial acetic acid, 3-[4-amino(hydroxyimino)methylphenyl]-5-[4-(1,2-diethoxycarbonylethyl)piperazinomethyl]oxazolidin-2-one, m.p. 186°, is obtained.
後処理
- customto give
出典と根拠
- ORDレコード
- ord-76c6d531face45d185a05c464261ac34
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05627197
関連ノート
読み込み中…