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Ammonium formate → HCID 178464891, 화합물

HRID 2246628
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HRID 2246628 반응식
[CH2:1]([NH:3][C:4](=[O:28])[C:5]1[CH:10]=[C:9]([C:11]2[CH:19]=[C:18]3[C:14]([C:15]([C:20]4[CH2:21][CH2:22][NH:23][CH2:24][CH:25]=4)=[N:16][NH:17]3)=[CH:13][CH:12]=2)[C:8]([CH3:26])=[C:7]([F:27])[CH:6]=1)[CH3:2].C([O-])=O.[NH4+]>[Pd].C(O)C>[CH2:1]([NH:3][C:4](=[O:28])[C:5]1[CH:10]=[C:9]([C:11]2[CH:19]=[C:18]3[C:14]([C:15]([CH:20]4[CH2:21][CH2:22][NH:23][CH2:24][CH2:25]4)=[N:16][NH:17]3)=[CH:13][CH:12]=2)[C:8]([CH3:26])=[C:7]([F:27])[CH:6]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 58899619HCID 58899619, 화합물2회

생성물 1

HCID 178464891HCID 178464891, 화합물수율 88.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

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온도
90 °C

실험 절차

A mixture of N-ethyl-3-fluoro-4-methyl-5-[3-(1,2,3,6-tetrahydro-4-pyridinyl)-1H-indazol-6-yl]benzamide (Intermediate 21, 100 mg), 10% palladium on carbon (20 mg) and ammonium formate (50 mg) in ethanol (10 mL) was stirred at 90° C. for 1 h under nitrogen. The catalyst was removed by filtration and the filtrate was concentrated under vacuum. The product was dissolved in methanol and eluted through an SCX ion exchange cartridge. Elution with a solution of ammonia (0.88) in methanol gave the title compound as a white solid (89 mg).

후처리

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under vacuum
  3. dissolutionThe product was dissolved in methanol
  4. washeluted through an SCX ion exchange cartridge
  5. washElution with a solution of ammonia (0.88) in methanol

출처 및 근거

ORD 기록
ord-132ca0880cab4604ae04c25033c0952d
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07687532B2

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