Sodium Hydroxide → 5-Oxazol-4-yl-thiophene-3-carboxylic acid

HRID 2068664

反応式

HRID 2068664 の反応式
C[O:2][C:3]([C:5]1[CH:9]=[C:8]([C:10]2[N:11]=[CH:12][O:13][CH:14]=2)[S:7][CH:6]=1)=[O:4].[OH-].[Na+]>CO>[O:13]1[CH:14]=[C:10]([C:8]2[S:7][CH:6]=[C:5]([C:3]([OH:4])=[O:2])[CH:9]=2)[N:11]=[CH:12]1

参加物

4

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 581102445-Oxazol-4-yl-thiophene-3-carboxylic acid methyl ester

生成物 1

HCID 581102215-Oxazol-4-yl-thiophene-3-carboxylic acid収率 50%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5-Oxazol-4-yl-thiophene-3-carboxylic acid methyl ester (0.338 g, 1.62 mmol) was dissolved in methanol (3 mL) and sodium hydroxide (1 N, 2.1 mL) was added. The mixture was stirred at room temperature for 2 hours then a further amount of sodium hydroxide (1 N, 1 mL) was added and stirring continued overnight. The mixture was concentrated and the residue treated with HCl (1 N, 3.5 mL). The resultant precipitate was collected by filtration to give the title compound as a tan/off-white solid (0.158 g). The filtrate was passed through an SCX-2 cartridge (20 g) and concentrated to give a further amount of the title compound as a tan solid (0.078 g). LCMS m/z 196.13 [M+H]+ R. T.=3.22 min (Analytical Method 9).

後処理

  1. stirringstirring continued overnight
  2. concentrationThe mixture was concentrated
  3. additionthe residue treated with HCl (1 N, 3.5 mL)
  4. filtrationThe resultant precipitate was collected by filtration

出典と根拠

ORDレコード
ord-f502ff8750ca488aa0aebeac9f6aec7f
出典データセット
uspto-grants-2012_10
特許番号
US08299063B2

関連ノート

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