Triethylamine → methyl 4-fluoro-5-phenyl-1H-pyrrole-3-carboxylate

HRID 1012455

반응식

HRID 1012455 반응식
Cl[C:2]1[NH:3][C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:5]([F:11])[C:6]=1[C:7]([O:9][CH3:10])=[O:8].C(N(CC)CC)C>CO.[C].[Pd]>[F:11][C:5]1[C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:2][NH:3][C:4]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 66974454methyl 2-chloro-4-fluoro-5-phenyl-1H-pyrrole-3-carboxylate

생성물 1

HCID 66974524methyl 4-fluoro-5-phenyl-1H-pyrrole-3-carboxylate수율 86,784.898%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

Methyl 2-chloro-4-fluoro-5-phenyl-1H-pyrrole-3-carboxylate (0.92 mg), 10% palladium carbon (50% containing water, 0.20 g) and triethylamine (0.56 mL) were suspended in methanol (30 mL), and the mixture was stirred under a hydrogen atmosphere at room temperature for 2 hr. The reaction mixture was filtered through celite, and the insoluble material was washed with ethyl acetate. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=19:1→1:1) to give the title compound as a colorless solid (yield 0.69 g, 87%).

후처리

  1. filtrationThe reaction mixture was filtered through celite
  2. washthe insoluble material was washed with ethyl acetate
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=19:1→1:1)

출처 및 근거

ORD 기록
ord-4533ef72fef24f07a856e7e415b9f822
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977488B2

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