反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:23]=3[Cl:30])=[C:19]([CH2:31]Cl)[N:18]=[C:17]([N:33]3[CH2:38][CH2:37][O:36][CH2:35][CH2:34]3)[N:16]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[C:39]([O-])(=[O:42])[CH2:40][OH:41].[Na+].[Na]>C(O)CO>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:23]=3[Cl:30])=[C:19]([CH2:31][O:41][CH2:40][CH2:39][OH:42])[N:18]=[C:17]([N:33]3[CH2:34][CH2:35][O:36][CH2:37][CH2:38]3)[N:16]=2)(=[O:12])=[O:13])=[CH:9][CH:10]=1)([CH3:3])([CH3:2])[CH3:4]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 80 °C
実験手順
1 g of 4-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide was added to a sodium glycolate solution from 2.5 g of ethylene glycol and 0.12 g of sodium. The reaction mixture was stirred at 80° C. under argon for 72 hours. Thereafter, the ethylene glycol was distilled off and the residue was partitioned between ethyl acetate and 1 N hydrochloric acid. The organic phase was washed with water, dried over sodium sulphate and the solvent was distilled off. The residue was chromatographed over silica gel with ether. There was obtained 0.85g of 4-tert-butyl-N-[5-(2-chloro-5methoxy-phenoxy)-6-(2-hydroxy-ethoxymethyl)-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide. m.p 162°-164° C., MS: M=606.
後処理
- distillationThereafter, the ethylene glycol was distilled off
- customthe residue was partitioned between ethyl acetate and 1 N hydrochloric acid
- washThe organic phase was washed with water
- dry with materialdried over sodium sulphate
- distillationthe solvent was distilled off
- customThe residue was chromatographed over silica gel with ether
出典と根拠
- ORDレコード
- ord-8af9041743f64ffb915679f0890fb30c
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05420129
関連ノート
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