Cesium carbonate → Methyl 3-(difluoromethoxy)-4-nitrobenzoate

HRID 1804671노트

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HRID 1804671 반응식
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-:12])=[O:11])=[C:6]([OH:13])[CH:5]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[F:21][CH:22]([F:24])I>CN(C=O)C>[F:21][CH:22]([F:24])[O:13][C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][C:7]=1[N+:10]([O-:12])=[O:11])[C:3]([O:2][CH3:1])=[O:14]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 294866Methyl 3-hydroxy-4-nitrobenzoateHCID 2775155Difluoro(iodo)methane

생성물 1

HCID 57969921Methyl 3-(difluoromethoxy)-4-nitrobenzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a cooled solution of 1 g of methyl-3-hydroxy-4-nitrobenzoate, 3.31 g of cesium carbonate in 20 mL of DMF, was carefully added 1.5 equivalents of difluoroiodomethane. The reaction was allowed to warm to room temperature and followed by TLC. Upon completion of the reaction, the mixture was concentrated and purified by silica get chromatography to give 1.2 g of methyl 3-(difluoromethoxy)-4-nitrobenzoate.

후처리

  1. customUpon completion of the reaction
  2. concentrationthe mixture was concentrated
  3. custompurified by silica
  4. customget chromatography

출처 및 근거

ORD 기록
ord-66544f61697a4cf2845067c944d467ee
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354420B2

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