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

HRID 876088노트

반응식

HRID 876088 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-69186a53844a41978c24028b3943d43c
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08986654B2

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