Hydrochloric Acid → 3-{4-[4-(2,4,6-Trimethylphenyl)piperazine-1-carbonyl]phenyl}oxazolidin-2-one

HRID 1804163

反応式

[O:1]=[C:2]1[N:6]([C:7]2[CH:17]=[CH:16][C:10]([C:11]([O:13]CC)=O)=[CH:9][CH:8]=2)[CH2:5][CH2:4][O:3]1.[OH-].[Na+].Cl.[CH3:21][C:22]1[CH:27]=[C:26]([CH3:28])[CH:25]=[C:24]([CH3:29])[C:23]=1[N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1.O.[Cl-].COC1N=C(OC)N=C([N+]2(C)CCOCC2)N=1>C(O)C>[CH3:29][C:24]1[CH:25]=[C:26]([CH3:28])[CH:27]=[C:22]([CH3:21])[C:23]=1[N:30]1[CH2:31][CH2:32][N:33]([C:11]([C:10]2[CH:9]=[CH:8][C:7]([N:6]3[CH2:5][CH2:4][O:3][C:2]3=[O:1])=[CH:17][CH:16]=2)=[O:13])[CH2:34][CH2:35]1

参加物

反応条件

温度: 50 °C

実験手順

To ethyl 4-(-2-oxooxazolidin-3-yl)benzoate (0.235 g) described in Preparation Example 12 were added 1 M aqueous sodium hydroxide solution (1.3 mL) and ethanol (5 mL), and the mixture was stirred at 50° C. 1N hydrochloric acid (1.3 mL) was added, 1-(2,4,6-trimethylphenyl)piperazine (0.215 g) and 4-(4,6-dimethoxy[1.3.5]triazin-2-yl)-4-methylmorpholinium chloride hydrate (0.277 g) were added, and the mixture was stirred at room temperature overnight. The mixture was extracted with ethyl acetate, washed with saturated brine, and the solvent was evaporated. The residue was purified by HPLC (ODS, 0.05% TFA aqueous solution-acetonitrile) to give the title compound (37.7 mg).

後処理

stirringthe mixture was stirred at room temperature overnight
extractionThe mixture was extracted with ethyl acetate
washwashed with saturated brine
customthe solvent was evaporated
customThe residue was purified by HPLC (ODS, 0.05% TFA aqueous solution-acetonitrile)

出典と根拠

ORDレコード: ord-540f18ada2da4cee81800e4aebeff0b0
出典データセット: uspto-grants-2013_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08354401B2

反応式

参加物

反応物 5

生成物 1

試薬・触媒・溶媒 1

反応条件

実験手順

後処理

出典と根拠

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