Methyl iodide → Methyl 2-bromo-6-methylbenzoate

HRID 1097976

反応式

HRID 1097976 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:3]=1[C:4]([OH:6])=[O:5].CI.[C:14](=O)([O-])O.[K+]>CN(C=O)C>[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:3]=1[C:4]([O:6][CH3:14])=[O:5]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 516893Potassium BicarbonateHCID 27355892-Bromo-6-methylbenzoic acid

生成物 1

HCID 11564857Methyl 2-bromo-6-methylbenzoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-bromo-6-methylbenzoic acid (5.02 g) and methyl iodide (2.9 mL) in N,N′-dimethylformamide (30 mL) was added powdered potassium hydrogen carbonate (4.67 g). The mixture was stirred at ambient temperature for 16 hours and concentrated. The concentrate was partitioned between ethyl acetate and water. The extract was washed with brine and concentrated, and the concentrate was purified by flash chromatography on silica gel with 60% ethyl acetate in hexanes.

後処理

  1. concentrationconcentrated
  2. customThe concentrate was partitioned between ethyl acetate and water
  3. washThe extract was washed with brine
  4. concentrationconcentrated
  5. customthe concentrate was purified by flash chromatography on silica gel with 60% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-95ffc6b7216c47e0afcf67899bff3076
出典データセット
uspto-grants-2012_03
特許番号
US08143284B2

関連ノート

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