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

HRID 1804671ノート

反応式

HRID 1804671 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-66544f61697a4cf2845067c944d467ee
出典データセット
uspto-grants-2013_01
特許番号
US08354420B2

反応ノート

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