Sodium Hydroxide → Benzoic Acid

HRID 2220376ノート

反応式

HRID 2220376 の反応式
C(OC(N(C[C@H](O)C1C=CC=CC=1)CCC1C=CC([C:17]2[CH:22]=[CH:21][C:20]([C:23]([O:25]C)=[O:24])=[C:19](C3SC=CC=3)[CH:18]=2)=CC=1)=O)(C)(C)C.[OH-].[Na+]>CO>[C:23]([OH:25])(=[O:24])[C:20]1[CH:21]=[CH:22][CH:17]=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 69103883HCID 69103883、化合物

生成物 1

HCID 243Benzoic Acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

To a solution of methyl 4′-[2-[(tert-butoxycarbonyl)-[(2R)-2-hydroxy-2-phenylethyl]amino]ethyl]-3-(2-thienyl)-4-bipheylcarboxylate (188 mg) in methanol (3.3 ml) was added 1N aqueous sodium hydroxide solution (1.0 ml), and the mixture was stirred at 40° C. for 3 hours. The solvent was removed by evaporation, and the aqueous solution was acidified with 1N aqueous hydrochloride solution and extracted with ethyl acetate (30 ml×2). The combined organic layers were washed with water and brine, dried over magnesium sulfate and evaporated under reduced pressure to give a benzoic acid product. To a solution of the product in ethyl acetate (1.0 ml) was added 4N hydrogen chloride in ethyl acetate (1.0 ml), and the mixture was stirred at room temperature for 12 hours. The resultant solid was collected by filtration and dried to give 4′-[2-[[(2R)-2-hydroxy-2-phenylethyl]amino]ethyl]-3-(2-thienyl)-4-biphenylcarboxylic acid hydrochloride (139 mg).

後処理

  1. customThe solvent was removed by evaporation
  2. extractionextracted with ethyl acetate (30 ml×2)
  3. washThe combined organic layers were washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-e7800ecd06ee4df1be433138b8291580
出典データセット
uspto-grants-2008_08
特許番号
US07417060B2

反応ノート

読み込み中…