Sodium Hydroxide → HCID 84655455、化合物

HRID 1478894ノート

反応式

HRID 1478894 の反応式
[CH3:1][N:2]1[C:10]2[CH:9]=[C:8]([C:11]([O:13]C)=[O:12])[N:7]=[CH:6][C:5]=2[CH:4]=[CH:3]1.[OH-].[Na+]>CO.[Cl-].[Na+].O>[CH3:1][N:2]1[C:10]2[CH:9]=[C:8]([C:11]([OH:13])=[O:12])[N:7]=[CH:6][C:5]=2[CH:4]=[CH:3]1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 86674844HCID 86674844、化合物

生成物 1

HCID 84655455HCID 84655455、化合物収率 83%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
0 °C

実験手順

In a 500 mL pear flask was added methyl 1-methyl-1H-pyrrolo[3,2-c]pyridine-6-carboxylate (1B, 14 g, 71 mmol) in methanol (71.0 ml). At 0° C. was added 1N sodium hydroxide solution (140 ml, 140 mmol). This was then stirred at 0° C. for 1 h, when the reaction was complete. Brine (25 ml) was added and methanol was removed in vacuo. The aqueous mixture was washed twice with EtOAc. The aqueous layer was then acidified to pH 4; the resulting precipitate was collected on a fritted glass funnel and dried overnight under a stream of nitrogen to give the desired product 1-methyl-1H -pyrrolo[3,2-c]pyridine-6-carboxylic acid (1C, 10 g, 83% yield) as an off white powder. This was used in next step without further purification.

後処理

  1. custommethanol was removed in vacuo
  2. washThe aqueous mixture was washed twice with EtOAc
  3. customthe resulting precipitate was collected on a fritted glass funnel
  4. customdried overnight under a stream of nitrogen

出典と根拠

ORDレコード
ord-e8019b4abca249afb374208a3e16ca63
出典データセット
uspto-grants-2016_08
特許番号
US09403819B2

反応ノート

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