Triethylamine → Methyl 2-chloro-2-(2-fluoro-4,5-dimethoxyphenyl)acetate

HRID 1667596ノート

反応式

HRID 1667596 の反応式
[F:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([O:10][CH3:11])=[CH:4][C:3]=1[CH:12](O)[C:13]([O:15][CH3:16])=[O:14].C(N(CC)CC)C.S([Cl:29])(C)(=O)=O>C(Cl)Cl>[Cl:29][CH:12]([C:3]1[CH:4]=[C:5]([O:10][CH3:11])[C:6]([O:8][CH3:9])=[CH:7][C:2]=1[F:1])[C:13]([O:15][CH3:16])=[O:14]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 57448188Methyl 2-(2-fluoro-4,5-dimethoxyphenyl)-2-hydroxyacetate

生成物 1

HCID 57448189Methyl 2-chloro-2-(2-fluoro-4,5-dimethoxyphenyl)acetate収率 89%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 7A (280 mg, 1.2 mmol) in CH2Cl2 (5 mL) at 0° C. was added triethylamine (0.42 mL, 3.0 mmol) followed by mesyl chloride (0.12 mL, 1.5 mmol). After stirring at rt overnight, the reaction was filtered, concentrated and purified via silica gel chromatography (0-30% ethyl acetate/hexanes) to provide 7B (268 mg, 89%).

後処理

  1. filtrationthe reaction was filtered
  2. concentrationconcentrated
  3. custompurified via silica gel chromatography (0-30% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-db2382aa09d64da395f4f001bfb2adf5
出典データセット
uspto-grants-2011_10
特許番号
US08044242B2

反応ノート

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