Sodium Hydroxide → HCID 84655455, 화합물

HRID 1478894노트

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HRID 1478894 반응식
[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

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 86674844HCID 86674844, 화합물

생성물 1

HCID 84655455HCID 84655455, 화합물수율 83%

시약·촉매·용매 2

HCID 887Methanol용매HCID 57417360Sodium chloride; water용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e8019b4abca249afb374208a3e16ca63
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403819B2

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