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

HRID 1012455

反応式

HRID 1012455 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-4533ef72fef24f07a856e7e415b9f822
出典データセット
uspto-grants-2011_07
特許番号
US07977488B2

関連ノート

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