Hydrochloric Acid → [[2-[(4-Acetyl-3-hydroxy-2-propylbenzyl)thio]-pyrimidin-4-yl]oxy]acetic acid

HRID 2107102ノート

反応式

HRID 2107102 の反応式
[C:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][S:9][C:10]2[N:15]=[C:14]([O:16][CH2:17][C:18]([O:20]CC)=[O:19])[CH:13]=[CH:12][N:11]=2)=[C:6]([CH2:25][CH2:26][CH3:27])[C:5]=1[OH:28])(=[O:3])[CH3:2].[OH-].[Na+].C(OCC)(=O)C.Cl>CO>[C:1]([C:4]1[CH:24]=[CH:23][C:7]([CH2:8][S:9][C:10]2[N:15]=[C:14]([O:16][CH2:17][C:18]([OH:20])=[O:19])[CH:13]=[CH:12][N:11]=2)=[C:6]([CH2:25][CH2:26][CH3:27])[C:5]=1[OH:28])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 14798Sodium Hydroxide2 回HCID 14053136Ethyl [[2-[(4-acetyl-3-hydroxy-2-propylbenzyl)thio]-pyrimidin-4-yl]oxy]acetate

生成物 1

HCID 14053137[[2-[(4-Acetyl-3-hydroxy-2-propylbenzyl)thio]-pyrimidin-4-yl]oxy]acetic acid収率 35.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

In 2 ml of 90% methanol was dissolved 0.06 g of ethyl [[2-[(4-acetyl-3-hydroxy-2-propylbenzyl)thio]-pyrimidin-4-yl]oxy]acetate obtained in Example 15 with heating at 60° C. Further 1 ml of a 1N aqueous sodium hydroxide solution was added to the solution followed by stirring at 60° C. for 15 minutes. An aqueous sodium hydroxide solution and ethyl acetate were added to the reaction mixture to fractionate. The aqueous phase was made acidic with 2N hydrochloric acid and extracted with ethyl acetate. The extract was washed with water and then dried over anhydrous magnesium sulfate. The solvent was then distilled off. The thus obtained solid was recrystallized from isopropyl alcohol to give 0.02 g of [[2-[(4-acetyl-3-hydroxy-2-propylbenzyl)thio]-pyrimidin-4-yl]oxy]acetic acid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was then distilled off
  5. customThe thus obtained solid was recrystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-ff3cf864f4d34372809738c74375b8f9
出典データセット
uspto-grants-1990_06
特許番号
US04933348

反応ノート

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