Sodium Hydroxide → 3-Phenoxy-3-phenyl-2-(4,6-dimethoxy-2-pyrimidinyl)oxybutyric acid

HRID 378364ノート

反応式

HRID 378364 の反応式
[O:1]([C:8]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([CH3:25])[CH:9]([O:14][C:15]1[N:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([O:23][CH3:24])[N:16]=1)[C:10]([O:12]C)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>CO.C1COCC1>[O:1]([C:8]([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)([CH3:25])[CH:9]([O:14][C:15]1[N:16]=[C:17]([O:23][CH3:24])[CH:18]=[C:19]([O:21][CH3:22])[N:20]=1)[C:10]([OH:12])=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 15766825Methyl 2-((4,6-Dimethoxypyrimidin-2-yl)oxy)-3-phenoxy-3-phenylbutanoate

生成物 1

HCID 152922993-Phenoxy-3-phenyl-2-(4,6-dimethoxy-2-pyrimidinyl)oxybutyric acid収率 79.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

1.3 g of methyl 3-phenoxy-3-phenyl-2-(4,6-dimethoxy-2-pyrimidinyl)oxybutyrate (Example 6 change to 42) are dissolved in 20 ml of MeOH and 40 ml of THF, and 3.7 g of 10% NaOH solution are added. The mixture is stirred at 60° C. for 6 hours and at room temperature for 12 hours, the solvent is removed by distillation under reduced pressure, and the residue is taken up in 100 ml of water. Unreacted ester is extracted with ethyl acetate. The aqueous phase is then adjusted to pH 1-2 with dilute hydrochloric acid and extracted with ethyl acetate. Drying over magnesium sulfate and removal of the solvent by distillation result in 1.0 g of a white powder.

後処理

  1. customthe solvent is removed by distillation under reduced pressure
  2. extractionUnreacted ester is extracted with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. dry with materialDrying over magnesium sulfate and removal of the solvent by distillation

出典と根拠

ORDレコード
ord-3d3dc731e6354698b23bee6d73931025
出典データセット
uspto-grants-2000_02
特許番号
US06030975

反応ノート

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