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

HRID 1438181ノート

反応式

HRID 1438181 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 139A (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 139B (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-3da6bb0fa6c04fc6bfa2205279827696
出典データセット
uspto-grants-2009_11
特許番号
US07622585B2

反応ノート

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