Sodium Hydroxide → 3-(4-Methoxy-1H-pyrazol-5-yl)-4-methylbenzoic acid

HRID 1488141ノート

反応式

HRID 1488141 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[N:5][NH:6][C:7]=1[C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][C:17]=1[CH3:18])[C:11]([O:13]C)=[O:12].[OH-].[Na+]>CO.O>[CH3:1][O:2][C:3]1[CH:4]=[N:5][NH:6][C:7]=1[C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][C:17]=1[CH3:18])[C:11]([OH:13])=[O:12]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 90030202Methyl 3-(4-methoxy-1H-pyrazol-5-yl)-4-methylbenzoate2 回

生成物 1

HCID 900296623-(4-Methoxy-1H-pyrazol-5-yl)-4-methylbenzoic acid収率 208.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

Into a 50-mL round-bottom flask, was placed a solution of methyl 3-(4-methoxy-1H-pyrazol-5-yl)-4-methylbenzoate (compound 244.6, 180 mg, 0.73 mmol) in methanol (4 mL). Sodium hydroxide (117 mg, 2.92 mmol) in water (2 mL) was added and the resulting solution was stirred for 3 h at 60° C., then concentrated under reduced pressure. The pH of the residue was adjusted to 1 with aqueous hydrogen chloride (1 M), then concentrated under reduced pressure. Methanol (5 mL) was added to the residue and the solids were filtered from the solution. The filtrate was concentrated under reduced pressure to obtain the title compound as a limit yellow solid (353 mg, crude).

後処理

  1. customInto a 50-mL round-bottom flask, was placed
  2. concentrationconcentrated under reduced pressure
  3. concentrationconcentrated under reduced pressure
  4. additionMethanol (5 mL) was added to the residue
  5. filtrationthe solids were filtered from the solution
  6. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-e565b459ca494b4caaae3d29ce9d7bc7
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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