Nitrogen → 2-(3-Acetyl-pyrazol-1-ylmethyl)-oxazole-4-carboxylic acid

HRID 1189391ノート

反応式

HRID 1189391 の反応式
N#N.C([O:5][C:6]([C:8]1[N:9]=[C:10]([CH2:13][N:14]2[CH:18]=[CH:17][C:16]([C:19](=[O:21])[CH3:20])=[N:15]2)[O:11][CH:12]=1)=[O:7])C.[OH-].[Na+]>C1COCC1.Cl>[C:19]([C:16]1[CH:17]=[CH:18][N:14]([CH2:13][C:10]2[O:11][CH:12]=[C:8]([C:6]([OH:7])=[O:5])[N:9]=2)[N:15]=1)(=[O:21])[CH3:20]

参加物

6

反応物 3

HCID 947NitrogenHCID 14798Sodium HydroxideHCID 671284172-(3-Acetyl-pyrazol-1-ylmethyl)-oxazole-4-carboxylic acid ethyl ester

生成物 1

HCID 671287672-(3-Acetyl-pyrazol-1-ylmethyl)-oxazole-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of 2-(3-acetyl-pyrazol-1-ylmethyl)-oxazole-4-carboxylic acid ethyl ester (137 mg, 0.52 mmol) in THF (5.0 mL) was treated at rt with 1N NaOH (2.5 mL, 2.5 mmol) and the reaction mixture was stirred for 3 h at rt. The reaction mixture was poured in 1N HCl (23 mL) and extracted with EA (50 mL). The org. extracts were dried over MgSO4, filtered, and the solvent was removed under reduced pressure to give the crude 2-(3-acetyl-pyrazol-1-ylmethyl)-oxazole-4-carboxylic acid as a deep brown foam. LC-MS-conditions 02: tR=0.64 min, [M+H]+=236.13.

後処理

  1. extractionextracted with EA (50 mL)
  2. dry with materialextracts were dried over MgSO4
  3. filtrationfiltered
  4. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-c845448f96bc494880a3c51bdb5455ab
出典データセット
uspto-grants-2014_03
特許番号
US08674111B2

反応ノート

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