Methyl iodide → Methyl 4,5-dichloro-2-methoxybenzoate

HRID 588827ノート

反応式

HRID 588827 の反応式
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.[C:14]([O-])([O-])=O.[K+].[K+].CI>CN(C=O)C>[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5]([C:6]([O:8][CH3:14])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 211803434,5-Dichloro-2-methoxybenzoic acid

生成物 1

HCID 23046708Methyl 4,5-dichloro-2-methoxybenzoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4,5-dichloro-2-methoxybenzoic acid (8.2 g, 37 mmol) and K2CO3 (11.8 g, 111 mmol) in DMF (100 mL), CH3I (6.3 g, 44 mmol) was added dropwise and the resulting mixture was stirred at room temperature for 16 h. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with water and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=10:1) to afford the desired product.

後処理

  1. additionwas added dropwise
  2. customThe mixture was partitioned between ethyl acetate and water
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-57eba321c9ee402e82750a7166ee683d
出典データセット
uspto-grants-2016_01
特許番号
US09227978B2

反応ノート

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