Sodium Hydroxide → 3-Acetyl-4-(2-isopropylphenyl)-6-methyl-1-carboxymethyl-2-pyridinone

HRID 398376ノート

反応式

HRID 398376 の反応式
[C:1]([C:4]1[C:5](=[O:26])[N:6]([CH2:20][C:21]([O:23]CC)=[O:22])[C:7]([CH3:19])=[CH:8][C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH:16]([CH3:18])[CH3:17])(=[O:3])[CH3:2].[OH-].[Na+]>C(O)C>[C:1]([C:4]1[C:5](=[O:26])[N:6]([CH2:20][C:21]([OH:23])=[O:22])[C:7]([CH3:19])=[CH:8][C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH:16]([CH3:18])[CH3:17])(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 230001623-Acetyl-4-(2-isopropylphenyl)-6-methyl-1-ethoxycarbonylmethyl-2-pyridinone

生成物 1

HCID 230001833-Acetyl-4-(2-isopropylphenyl)-6-methyl-1-carboxymethyl-2-pyridinone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of 3-acetyl-4-(2-isopropylphenyl)-6-methyl-1-ethoxycarbonylmethyl-2-pyridinone from step 3 of Example XX (0.20 g, 0.56 mmol) in ethanol (4 mL) was added aqueous NaOH (0.62 mL of a 1.0 N solution, 0.62 mmol). The resulting solution was stirred at ambient temperature for 2 h and the solvent was removed in vacuo. The residue was partitioned between EtOAc and 1.0 N aqueous HCl. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic extracts were dried over Na2SO4, filtered, and concentrated in vacuo to give the title compound (HPLC RT=18.11 min, method B).

後処理

  1. customthe solvent was removed in vacuo
  2. customThe residue was partitioned between EtOAc and 1.0 N aqueous HCl
  3. customThe organic phase was separated
  4. extractionthe aqueous phase was extracted with EtOAc
  5. dry with materialThe combined organic extracts were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bdd5c6c64fa04af9a393582da96f25e1
出典データセット
uspto-grants-2003_08
特許番号
US06610692B1

反応ノート

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