Sodium Hydroxide → HCID 21942438、化合物

HRID 2216771ノート

反応式

HRID 2216771 の反応式
C[O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:7]=[C:6]([F:16])[CH:5]=1.[OH-].[Na+]>CO>[F:16][C:6]1[CH:5]=[C:4]([CH:9]=[C:8]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:7]=1)[C:3]([OH:17])=[O:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 21942429Methyl-3-fluoro-5-(3-pyridyl)benzoate

生成物 1

HCID 21942438HCID 21942438、化合物収率 117.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a 100 ml round bottom flask equipped with stir bar added Methyl-3-fluoro-5-(3-pyridyl)benzoate (0.92 g, 3.93 mmol), methanol (10 ml) and sodium hydroxide (5.89 ml, 5.89 mmol, 1N aqueous). Stirred the resulting mixture at 50° C. for 2 h. The reaction mixture was cooled to room temperature, concentrated in-vacuo and the residue was dissolved in methanol (20 ml). To this mixture added hydrochloric acid (1N diethyl ether) dropwise and stirred at room temperature for 10 min. The reaction mixture was concentrated in-vacuo and the residue was triturated with diethyl ether to provide the crude hydrochloride salt of title compound (1.00 g) as an off white solid.

後処理

  1. customIn a 100 ml round bottom flask equipped
  2. stirringStirred the resulting mixture at 50° C. for 2 h
  3. concentrationconcentrated in-vacuo
  4. dissolutionthe residue was dissolved in methanol (20 ml)
  5. additionTo this mixture added hydrochloric acid (1N diethyl ether) dropwise
  6. stirringstirred at room temperature for 10 min
  7. concentrationThe reaction mixture was concentrated in-vacuo
  8. customthe residue was triturated with diethyl ether

出典と根拠

ORDレコード
ord-36782e45cb50431e80eb316b1e128bda
出典データセット
uspto-grants-2006_09
特許番号
US07112595B2

反応ノート

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