Dimethylformamide → Methyl 1-(difluoromethyl)pyrrole-2-carboxylate

HRID 876088ノート

反応式

HRID 876088 の反応式
[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([O:8][CH3:9])=[O:7].[F:10][CH:11]([F:13])I.CN(C=O)C.[H-].[Na+]>O>[F:10][CH:11]([F:13])[N:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([O:8][CH3:9])=[O:7]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 136930Methyl pyrrole-2-carboxylateHCID 2775155Difluoro(iodo)methane

生成物 1

HCID 86709246Methyl 1-(difluoromethyl)pyrrole-2-carboxylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Was prepared from stirred a mixture of methyl 1H-pyrrole-2-carboxylate (3.04 g, 23.5 mmol), difluoroiodomethane (4.4 g, 24.7 mmol) and DMF (40 ml). Sodium hydride (1.41 g, 35.2 mmol) was added in portions during 30 minutes. The mixture was stirred for additional 15 minutes. Water (50 ml) was added and the mixture was extracted with dichloromethane. The mixture was purified by silica gel chromatography, using dichloromethane as solvent. The product was dried and evaporated. Yield 3.21 g (78%).

後処理

  1. customWas prepared
  2. stirringThe mixture was stirred for additional 15 minutes
  3. extractionthe mixture was extracted with dichloromethane
  4. customThe mixture was purified by silica gel chromatography
  5. customThe product was dried
  6. customevaporated

出典と根拠

ORDレコード
ord-69186a53844a41978c24028b3943d43c
出典データセット
uspto-grants-2015_03
特許番号
US08986654B2

反応ノート

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